CN113981026A - High-purity glucosamine hydrochloride and preparation method thereof - Google Patents
High-purity glucosamine hydrochloride and preparation method thereof Download PDFInfo
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- CBOJBBMQJBVCMW-BTVCFUMJSA-N (2r,3r,4s,5r)-2-amino-3,4,5,6-tetrahydroxyhexanal;hydrochloride Chemical compound Cl.O=C[C@H](N)[C@@H](O)[C@H](O)[C@H](O)CO CBOJBBMQJBVCMW-BTVCFUMJSA-N 0.000 title claims abstract description 54
- 229960001911 glucosamine hydrochloride Drugs 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 78
- 240000008042 Zea mays Species 0.000 claims abstract description 61
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims abstract description 61
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims abstract description 61
- 235000005822 corn Nutrition 0.000 claims abstract description 61
- 238000000855 fermentation Methods 0.000 claims abstract description 30
- 230000004151 fermentation Effects 0.000 claims abstract description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000001914 filtration Methods 0.000 claims abstract description 26
- 241000894006 Bacteria Species 0.000 claims abstract description 25
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 claims abstract description 25
- 235000013922 glutamic acid Nutrition 0.000 claims abstract description 25
- 239000004220 glutamic acid Substances 0.000 claims abstract description 25
- 239000012043 crude product Substances 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 239000000047 product Substances 0.000 claims abstract description 15
- 238000000643 oven drying Methods 0.000 claims abstract description 14
- 238000010306 acid treatment Methods 0.000 claims abstract description 13
- 238000010992 reflux Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 11
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 7
- 230000001376 precipitating effect Effects 0.000 claims abstract description 7
- 238000005303 weighing Methods 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 48
- 239000002893 slag Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 240000004808 Saccharomyces cerevisiae Species 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 230000007062 hydrolysis Effects 0.000 claims description 6
- 238000006460 hydrolysis reaction Methods 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 239000012629 purifying agent Substances 0.000 claims description 6
- 235000013305 food Nutrition 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 241000196324 Embryophyta Species 0.000 abstract description 3
- MSWZFWKMSRAUBD-IVMDWMLBSA-N 2-amino-2-deoxy-D-glucopyranose Chemical compound N[C@H]1C(O)O[C@H](CO)[C@@H](O)[C@@H]1O MSWZFWKMSRAUBD-IVMDWMLBSA-N 0.000 abstract description 2
- 206010028391 Musculoskeletal Pain Diseases 0.000 abstract description 2
- 206010070834 Sensitisation Diseases 0.000 abstract description 2
- 210000001188 articular cartilage Anatomy 0.000 abstract description 2
- MSWZFWKMSRAUBD-UHFFFAOYSA-N beta-D-galactosamine Natural products NC1C(O)OC(CO)C(O)C1O MSWZFWKMSRAUBD-UHFFFAOYSA-N 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- 235000013376 functional food Nutrition 0.000 abstract description 2
- 229960002442 glucosamine Drugs 0.000 abstract description 2
- 201000008482 osteoarthritis Diseases 0.000 abstract description 2
- 230000001737 promoting effect Effects 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 230000008313 sensitization Effects 0.000 abstract description 2
- 230000008901 benefit Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 210000004185 liver Anatomy 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- MTDHILKWIRSIHB-UHFFFAOYSA-N (5-azaniumyl-3,4,6-trihydroxyoxan-2-yl)methyl sulfate Chemical compound NC1C(O)OC(COS(O)(=O)=O)C(O)C1O MTDHILKWIRSIHB-UHFFFAOYSA-N 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 208000007107 Stomach Ulcer Diseases 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 239000002246 antineoplastic agent Substances 0.000 description 1
- 229940041181 antineoplastic drug Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000001784 detoxification Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 201000005917 gastric ulcer Diseases 0.000 description 1
- 229960002849 glucosamine sulfate Drugs 0.000 description 1
- 150000002337 glycosamines Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- LPUQAYUQRXPFSQ-DFWYDOINSA-M monosodium L-glutamate Chemical compound [Na+].[O-]C(=O)[C@@H](N)CCC(O)=O LPUQAYUQRXPFSQ-DFWYDOINSA-M 0.000 description 1
- 235000013923 monosodium glutamate Nutrition 0.000 description 1
- 239000004223 monosodium glutamate Substances 0.000 description 1
- 235000019629 palatability Nutrition 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 201000003068 rheumatic fever Diseases 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/26—Preparation of nitrogen-containing carbohydrates
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H5/00—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium
- C07H5/04—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium to nitrogen
- C07H5/06—Aminosugars
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Bioinformatics & Cheminformatics (AREA)
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention belongs to the technical field of food and chemical industry, and particularly relates to high-purity glucosamine hydrochloride and a preparation method thereof, wherein the preparation method comprises the following steps: weighing corn grit, citric acid fermentation residue and glutamic acid bacteria residue according to a ratio; dividing the corn grit into two parts; mixing a part of corn residue with citric acid fermentation residue, performing acid treatment, and drying to obtain dry residue A; fermenting the other part of corn residue to obtain ethanol solution, mixing with glutamic acid bacteria residue, reflux extracting, filtering, oven drying to obtain dry residue B, and oven drying the filter residue to obtain dry residue C; mixing the obtained dry residues, and crushing to obtain a dry powder material; hydrolyzing the dry powder, filtering, and cooling and crystallizing the filtrate to obtain a glucosamine hydrochloride crude product; and (4) dissolving the crude product, decoloring, precipitating with alcohol, and drying to obtain the product. The product plant-derived glucosamine prepared by the invention has the characteristics of high purity and no alpha-shell sensitization source, and is an important medicine and functional food raw material for promoting the recovery of articular cartilage, relieving osteoarticular pain and assisting in treating osteoarthritis.
Description
Technical Field
The invention belongs to the technical field of food and chemical industry, and particularly relates to high-purity glucosamine hydrochloride and a preparation method thereof.
Background
Glucosamine hydrochloride is also called glucosamine hydrochloride. Has important physiological functions for human body, participates in detoxification of liver and kidney, and plays a role in resisting inflammation and protecting liver. Has good curative effect on treating rheumatic arthritis and gastric ulcer. Is a main raw material for synthesizing antibiotics and anticancer drugs, and can also be used in chemical industry, food, cosmetics and feed additives. The main effective component of the amino sugar capsule health care product sold in the market at present is glucosamine hydrochloride or glucosamine sulfate. Glucosamine hydrochloride is a fine chemical product, has high price and large market demand, is mostly prepared by hydrolyzing insect shells or carapace at high temperature at present, and has relatively limited source.
The corn grit is agricultural waste, and if the corn grit can be recycled, huge economic and social benefits can be generated.
The citric acid fermentation residue is the fermentation liquor squeezing waste of a citric acid plant. China is a world large country for citric acid production, the annual capacity is close to 100 ten thousand tons, and 1.5-2.0 tons of waste residues are discharged when 1 ton of citric acid is produced. Although some manufacturers dry the slope slag to prepare dry feed after drying and crushing, the pH value of the slope slag is about 2.5-3.0, and the slope slag is acidic and has poor palatability and is not popular.
The glutamic acid bacteria residues are main byproducts of the monosodium glutamate industry, millions of tons of glutamic acid bacteria residues are produced in China every year, and the glutamic acid bacteria residues are reused and are mostly used as feed and fertilizer at present, so that the generated utilization value is relatively low.
In the prior art, a method for preparing high-purity glucosamine hydrochloride by compounding citric acid fermentation residues and glutamic acid bacteria residues is lacked.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide high-purity glucosamine hydrochloride and a preparation method thereof.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a preparation method of high-purity glucosamine hydrochloride is characterized by comprising the following steps:
1) weighing corn grit, citric acid fermentation residue and glutamic acid bacteria residue according to a ratio; dividing corn grit into two parts, namely corn grit a and corn grit b;
2) mixing the corn residue a and the citric acid fermentation residue, adding water and hydrochloric acid, carrying out acid treatment for 3-5 hours at the temperature of 90-95 ℃, and drying to obtain dry residue A; placing the corn residue B in a fermentation container, adding yeast, fermenting under anaerobic condition, filtering to obtain ethanol solution, adding into glutamic acid bacteria residue, reflux extracting, filtering, oven drying to obtain dry residue B, and oven drying the filter residue to obtain dry residue C; mixing the obtained dry slag A, dry slag B and dry slag C, and crushing to obtain a dry powder material;
3) adding water and hydrochloric acid into the obtained dry powder in sequence, hydrolyzing for 3-5 hours at 18-22 ℃, filtering, and cooling and crystallizing the filtrate to obtain a glucosamine hydrochloride crude product;
4) and dissolving the obtained glucosamine hydrochloride crude product, decoloring, precipitating with alcohol, and drying to obtain a glucosamine hydrochloride product.
Further, in the preparation method of the high-purity glucosamine hydrochloride, in the step 1), the mass ratio of the corn grit, the citric acid fermentation residue and the glutamic acid bacteria residue is 10-15:3-5:2, and the mass ratio of the corn grit a to the corn grit b is 1-2: 1.
further, in the method for producing high-purity glucosamine hydrochloride as described above, in step 2), the volume concentration of hydrochloric acid is maintained at 2 to 3% during the acid treatment.
Further, in the method for preparing high-purity glucosamine hydrochloride, step 2), the dry powder has a mesh size of 30-50 meshes.
Further, in the method for preparing high-purity glucosamine hydrochloride as described above, in step 3), the volume concentration of hydrochloric acid is maintained at 28 to 32% during the hydrolysis.
Further, as the above-mentioned preparation method of high-purity glucosamine hydrochloride, in the step 4), the decoloring method is as follows: adding active carbon with a total mass of 3% of the crude product, refluxing for 20min, and filtering while hot.
Further, in the method for preparing high-purity glucosamine hydrochloride as described above, in step 4), the purifying agent used in the alcohol precipitation is methanol.
High-purity glucosamine hydrochloride is prepared by the preparation method.
The invention has the beneficial effects that:
the invention provides a preparation method of high-purity glucosamine hydrochloride, which is based on corn residue, citric acid fermentation residue and glutamic acid bacteria residue as raw materials, and has the advantages of less types and dosage of required reagents, and reduction of the preparation cost of the glucosamine hydrochloride; meanwhile, the prepared product, namely the plant-derived glucosamine has the characteristics of high purity, no alpha-shell sensitization source, no fishy smell and no heavy metal pollution, and is an important medicine and functional food raw material for promoting the recovery of articular cartilage, relieving osteoarticular pain and assisting in treating osteoarthritis.
Of course, it is not necessary for any one product that embodies the invention to achieve all of the above advantages simultaneously.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A preparation method of high-purity glucosamine hydrochloride comprises the following steps:
1) weighing corn grit, citric acid fermentation residue and glutamic acid bacteria residue according to a ratio; dividing corn grit into two parts, namely corn grit a and corn grit b; the mass ratio of the corn grit to the citric acid fermentation residue to the glutamic acid bacteria residue is 10-15:3-5:2, and the mass ratio of the corn grit a to the corn grit b is 1-2: 1;
2) mixing the corn residue a and the citric acid fermentation residue, adding water and hydrochloric acid, and carrying out acid treatment at 90-95 ℃ for 3-5 hours, wherein the volume concentration of the hydrochloric acid in the acid treatment process is kept at 2-3%; drying to obtain dry residue A; placing the corn residue B in a fermentation container, adding yeast, fermenting under anaerobic condition, filtering to obtain ethanol solution, adding into glutamic acid bacteria residue, reflux extracting, filtering, oven drying to obtain dry residue B, and oven drying the filter residue to obtain dry residue C; mixing the obtained dry slag A, dry slag B and dry slag C, and crushing to obtain a dry powder material, wherein the mesh number of the dry powder material is 30-50 meshes;
3) adding water and hydrochloric acid into the obtained dry powder in sequence, and hydrolyzing at 18-22 deg.C for 3-5 hr with hydrochloric acid volume concentration of 28-32% during hydrolysis; filtering, and cooling and crystallizing the filtrate to obtain a glucosamine hydrochloride crude product;
4) dissolving the obtained glucosamine hydrochloride crude product, and decoloring and alcohol precipitating after dissolving, wherein the decoloring method comprises the following steps: adding active carbon with a total mass of 3% of the crude product, refluxing for 20min, and filtering while the solution is hot; the purifying agent used for alcohol precipitation is methanol; and drying to obtain the glucosamine hydrochloride product.
The following embodiments are relevant to the present invention:
example 1
A preparation method of high-purity glucosamine hydrochloride comprises the following steps:
1) weighing corn grit, citric acid fermentation residue and glutamic acid bacteria residue according to a ratio; dividing corn grit into two parts, namely corn grit a and corn grit b; the mass ratio of the corn grit to the citric acid fermentation residue to the glutamic acid bacteria residue is 13:4:2, and the mass ratio of the corn grit a to the corn grit b is 1: 1;
2) mixing the corn residue a and the citric acid fermentation residue, adding water and hydrochloric acid, and carrying out acid treatment at 92 ℃ for 4 hours, wherein the volume concentration of the hydrochloric acid in the acid treatment process is kept to be 2%; drying to obtain dry residue A; placing the corn residue B in a fermentation container, adding yeast, fermenting under anaerobic condition, filtering to obtain ethanol solution, adding into glutamic acid bacteria residue, reflux extracting, filtering, oven drying to obtain dry residue B, and oven drying the filter residue to obtain dry residue C; mixing the obtained dry slag A, dry slag B and dry slag C, and crushing to obtain a dry powder material, wherein the mesh number of the dry powder material is 40 meshes;
3) adding water and hydrochloric acid into the obtained dry powder in sequence, and hydrolyzing for 4 hours at 20 ℃, wherein the volume concentration of the hydrochloric acid is kept at 30% in the hydrolysis process; filtering, and cooling and crystallizing the filtrate to obtain a glucosamine hydrochloride crude product;
4) dissolving the obtained glucosamine hydrochloride crude product, and decoloring and alcohol precipitating after dissolving, wherein the decoloring method comprises the following steps: adding active carbon with a total mass of 3% of the crude product, refluxing for 20min, and filtering while the solution is hot; the purifying agent used for alcohol precipitation is methanol; and drying to obtain the glucosamine hydrochloride product.
Example 2
A preparation method of high-purity glucosamine hydrochloride comprises the following steps:
1) weighing corn grit, citric acid fermentation residue and glutamic acid bacteria residue according to a ratio; dividing corn grit into two parts, namely corn grit a and corn grit b; the mass ratio of the corn grit to the citric acid fermentation residue to the glutamic acid bacteria residue is 10:3:2, and the mass ratio of the corn grit a to the corn grit b is 2: 1;
2) mixing the corn residue a and the citric acid fermentation residue, adding water and hydrochloric acid, and carrying out acid treatment at 90 ℃ for 3 hours, wherein the volume concentration of the hydrochloric acid in the acid treatment process is kept to be 3%; drying to obtain dry residue A; placing the corn residue B in a fermentation container, adding yeast, fermenting under anaerobic condition, filtering to obtain ethanol solution, adding into glutamic acid bacteria residue, reflux extracting, filtering, oven drying to obtain dry residue B, and oven drying the filter residue to obtain dry residue C; mixing the obtained dry slag A, dry slag B and dry slag C, and crushing to obtain a dry powder material, wherein the mesh number of the dry powder material is 50 meshes;
3) adding water and hydrochloric acid into the obtained dry powder in sequence, and hydrolyzing for 3 hours at 18 ℃, wherein the volume concentration of the hydrochloric acid is kept at 32% in the hydrolysis process; filtering, and cooling and crystallizing the filtrate to obtain a glucosamine hydrochloride crude product;
4) dissolving the obtained glucosamine hydrochloride crude product, and decoloring and alcohol precipitating after dissolving, wherein the decoloring method comprises the following steps: adding active carbon with a total mass of 3% of the crude product, refluxing for 20min, and filtering while the solution is hot; the purifying agent used for alcohol precipitation is methanol; and drying to obtain the glucosamine hydrochloride product.
Example 3
A preparation method of high-purity glucosamine hydrochloride comprises the following steps:
1) weighing corn grit, citric acid fermentation residue and glutamic acid bacteria residue according to a ratio; dividing corn grit into two parts, namely corn grit a and corn grit b; the mass ratio of the corn grit to the citric acid fermentation residue to the glutamic acid bacteria residue is 15:5:2, and the mass ratio of the corn grit a to the corn grit b is 2: 1;
2) mixing the corn residue a and the citric acid fermentation residue, adding water and hydrochloric acid, and carrying out acid treatment at 95 ℃ for 5 hours, wherein the volume concentration of the hydrochloric acid in the acid treatment process is kept to be 3%; drying to obtain dry residue A; placing the corn residue B in a fermentation container, adding yeast, fermenting under anaerobic condition, filtering to obtain ethanol solution, adding into glutamic acid bacteria residue, reflux extracting, filtering, oven drying to obtain dry residue B, and oven drying the filter residue to obtain dry residue C; mixing the obtained dry slag A, dry slag B and dry slag C, and crushing to obtain a dry powder material, wherein the mesh number of the dry powder material is 30 meshes;
3) adding water and hydrochloric acid into the obtained dry powder in sequence, and hydrolyzing for 5 hours at 22 ℃, wherein the volume concentration of the hydrochloric acid in the hydrolysis process is kept to be 28%; filtering, and cooling and crystallizing the filtrate to obtain a glucosamine hydrochloride crude product;
4) dissolving the obtained glucosamine hydrochloride crude product, and decoloring and alcohol precipitating after dissolving, wherein the decoloring method comprises the following steps: adding active carbon with a total mass of 3% of the crude product, refluxing for 20min, and filtering while the solution is hot; the purifying agent used for alcohol precipitation is methanol; and drying to obtain the glucosamine hydrochloride product.
Example 4
The glucosamine hydrochloride products obtained in the embodiments 1 to 3 are subjected to physicochemical detection according to an enterprise standard Q/330400NDK003-2020, and the requirements of WS1-XG-028-2001 glucosamine hydrochloride and GB16740 national standard health food for food safety and the requirements of the development of the enterprise on the products are made according to the enterprise standard Q/330400NDK 003-2020.
The results of the physical and chemical index measurements are shown in Table 1:
TABLE 1
For glucosamine hydrochloride products obtained in examples 1 to 3, the microbial detection was performed according to the test method provided by the general rule of chinese pharmacopoeia 1105/1106, and the test results are shown in table 2:
TABLE 2
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (8)
1. A preparation method of high-purity glucosamine hydrochloride is characterized by comprising the following steps:
1) weighing corn grit, citric acid fermentation residue and glutamic acid bacteria residue according to a ratio; dividing corn grit into two parts, namely corn grit a and corn grit b;
2) mixing the corn residue a and the citric acid fermentation residue, adding water and hydrochloric acid, carrying out acid treatment for 3-5 hours at the temperature of 90-95 ℃, and drying to obtain dry residue A; placing the corn residue B in a fermentation container, adding yeast, fermenting under anaerobic condition, filtering to obtain ethanol solution, adding into glutamic acid bacteria residue, reflux extracting, filtering, oven drying to obtain dry residue B, and oven drying the filter residue to obtain dry residue C; mixing the obtained dry slag A, dry slag B and dry slag C, and crushing to obtain a dry powder material;
3) adding water and hydrochloric acid into the obtained dry powder in sequence, hydrolyzing for 3-5 hours at 18-22 ℃, filtering, and cooling and crystallizing the filtrate to obtain a glucosamine hydrochloride crude product;
4) and dissolving the obtained glucosamine hydrochloride crude product, decoloring, precipitating with alcohol, and drying to obtain a glucosamine hydrochloride product.
2. The method for producing high-purity glucosamine hydrochloride according to claim 1, wherein: in the step 1), the mass ratio of the corn grit to the citric acid fermentation residue to the glutamic acid bacteria residue is 10-15:3-5:2, and the mass ratio of the corn grit a to the corn grit b is 1-2: 1.
3. the method for producing high-purity glucosamine hydrochloride according to claim 1, wherein: in the step 2), the volume concentration of the hydrochloric acid in the acid treatment process is kept to be 2-3%.
4. The method for producing high-purity glucosamine hydrochloride according to claim 1, wherein: in the step 2), the mesh number of the dry powder is 30-50 meshes.
5. The method for producing high-purity glucosamine hydrochloride according to claim 1, wherein: in the step 3), the volume concentration of the hydrochloric acid in the hydrolysis process is kept between 28 and 32 percent.
6. The method for producing high-purity glucosamine hydrochloride according to claim 1, wherein: in the step 4), the decoloring method comprises the following steps: adding active carbon with a total mass of 3% of the crude product, refluxing for 20min, and filtering while hot.
7. The method for producing high-purity glucosamine hydrochloride according to claim 1, wherein: in the step 4), the purifying agent used for alcohol precipitation is methanol.
8. A high-purity glucosamine hydrochloride produced by the production method according to any one of claims 1 to 7.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101487028A (en) * | 2009-02-18 | 2009-07-22 | 李红玉 | Process for producing ethanol from potato residue |
| US20120095204A1 (en) * | 2010-10-14 | 2012-04-19 | Bai Jianguo | Method to prepare d-glucosamine hydrochloride |
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| CN101487028A (en) * | 2009-02-18 | 2009-07-22 | 李红玉 | Process for producing ethanol from potato residue |
| US20120095204A1 (en) * | 2010-10-14 | 2012-04-19 | Bai Jianguo | Method to prepare d-glucosamine hydrochloride |
| CN102464679A (en) * | 2010-11-04 | 2012-05-23 | 江苏江山制药有限公司 | Production process for preparing high-purity D-glucosamine hydrochloride from citric acid fermentation residues |
| CN105603024A (en) * | 2016-03-08 | 2016-05-25 | 扬州日兴生物科技股份有限公司 | Method for extracting glucosamine from corn grits through bioconversion |
| CN106188168A (en) * | 2016-07-18 | 2016-12-07 | 山东师范大学 | Utilize the method that the dreg producing glutamic acid prepares glucosamine hydrochloride |
| CN108956838A (en) * | 2018-08-07 | 2018-12-07 | 江苏双林海洋生物药业有限公司 | The detection method of aminoglucose sugared content in agricultural product |
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