CN101941974B - Purification method of riboflavin - Google Patents
Purification method of riboflavin Download PDFInfo
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- CN101941974B CN101941974B CN2010102930007A CN201010293000A CN101941974B CN 101941974 B CN101941974 B CN 101941974B CN 2010102930007 A CN2010102930007 A CN 2010102930007A CN 201010293000 A CN201010293000 A CN 201010293000A CN 101941974 B CN101941974 B CN 101941974B
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- gram
- vitamin
- riboflavin
- add
- deionized water
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- AUNGANRZJHBGPY-SCRDCRAPSA-N Riboflavin Chemical compound OC[C@@H](O)[C@@H](O)[C@@H](O)CN1C=2C=C(C)C(C)=CC=2N=C2C1=NC(=O)NC2=O AUNGANRZJHBGPY-SCRDCRAPSA-N 0.000 title claims abstract description 47
- 235000019192 riboflavin Nutrition 0.000 title claims abstract description 42
- 239000002151 riboflavin Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000000746 purification Methods 0.000 title claims abstract description 19
- AUNGANRZJHBGPY-UHFFFAOYSA-N D-Lyxoflavin Natural products OCC(O)C(O)C(O)CN1C=2C=C(C)C(C)=CC=2N=C2C1=NC(=O)NC2=O AUNGANRZJHBGPY-UHFFFAOYSA-N 0.000 title abstract 5
- 229960002477 riboflavin Drugs 0.000 title abstract 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 26
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 9
- GTSHREYGKSITGK-UHFFFAOYSA-N sodium ferrocyanide Chemical compound [Na+].[Na+].[Na+].[Na+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] GTSHREYGKSITGK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 235000012247 sodium ferrocyanide Nutrition 0.000 claims abstract description 9
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 9
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 9
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 235000011167 hydrochloric acid Nutrition 0.000 claims description 12
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 8
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 8
- 150000002978 peroxides Chemical class 0.000 claims description 8
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 8
- 239000012982 microporous membrane Substances 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000012043 crude product Substances 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 4
- 238000005374 membrane filtration Methods 0.000 claims description 4
- 239000012452 mother liquor Substances 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 235000011147 magnesium chloride Nutrition 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 2
- 239000002253 acid Substances 0.000 abstract 2
- 239000000047 product Substances 0.000 abstract 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 abstract 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 1
- 239000000706 filtrate Substances 0.000 abstract 1
- 229960002163 hydrogen peroxide Drugs 0.000 abstract 1
- 238000011085 pressure filtration Methods 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- 239000000264 sodium ferrocyanide Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 2
- 230000004060 metabolic process Effects 0.000 description 2
- 206010063409 Acarodermatitis Diseases 0.000 description 1
- 206010010741 Conjunctivitis Diseases 0.000 description 1
- 208000006069 Corneal Opacity Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 206010028116 Mucosal inflammation Diseases 0.000 description 1
- 241000447727 Scabies Species 0.000 description 1
- 208000028990 Skin injury Diseases 0.000 description 1
- 206010047612 Vitamin B2 deficiency Diseases 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 201000007590 ariboflavinosis Diseases 0.000 description 1
- 230000037396 body weight Effects 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 231100000269 corneal opacity Toxicity 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 210000000214 mouth Anatomy 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 208000004223 riboflavin deficiency Diseases 0.000 description 1
- 208000005687 scabies Diseases 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000009978 visual deterioration Effects 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
- 239000001060 yellow colorant Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a purification method of riboflavin, which comprises the following steps: dissolving crude riboflavin products in a hydrochloric acid solution, sequentially adding oxydol, zinc sulfate and sodium ferrocyanide, lauryl sodium sulfate, magnesium chloride, activated carbon and diatomite to the riboflavin-dissolved hydrochloric acid solution, carrying out air pump filtration or pressure filtration on the riboflavin-dissolved hydrochloric acid solution after spreading two layers of acid resistant cloths in a vacuum filter, sequentially filtering the obtained filtrate by an acid resistant microporous-film filter for three times, adding de-ionized water to a crystallizing tank, heating with steam, drying, crushing and sieving. The invention relates to a production process for purifying crude riboflavin products and has the advantages of simple purification process, convenient operation, low cost, low impurity content after purification and the like, and the riboflavin content can be more than 98% after purification.
Description
Technical field
The invention belongs to medical manufacturing technology field, a kind of specifically vitamin G process for purification refine.
Background technology
Vitamin G (Wei ShengsuB2) has health protection and medicine effect, thereby is widely used as food and feed additive, and it also can be used as the yellow colorants of food.In the prior art with compound method and various not to fermentation process, use suitable Separation and Recovery and purification step can make the vitamin G that obtains satisfy the specification of quality that some are slightly carried, for example be used for animal-feed.But major part can't satisfy the purifying requirement, in the food especially for the people.Wei ShengsuB2 is participated in the utilization of carbohydrate in body metabolism; Vitamin B2 deficiency and inflammation overworked with mucosal inflammation, the skin scabies of oral cavity and throat and similar skin injury, conjunctiva inflammation, visual deterioration and the corneal opacity etc. are relevant; In baby and children, as the B2 that is deficient in vitamin can cause growth to stop to reduce with body weight.Therefore Wei ShengsuB2 plays an important role in body metabolism.How to provide a kind of can be with vitamin G purifying crude and the high vitamin G process for purification refine of purification degrees.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art, a kind of easy and simple to handle, with low cost and vitamin G process for purification refine that purification degrees is high is provided.
The objective of the invention is to realize like this: a kind of vitamin G process for purification refine comprises following process step:
(1) temperature be under 55 ℃～60 ℃ the agitation condition with every gram vitamin G dissolving crude product in 2.5 milliliters～3.0 milliliters of the technical hydrochloric acids of concentration >=30%;
(2) in vitamin G dissolving with hydrochloric acid liquid, add ydrogen peroxide 50, zinc sulfate, yellow prussiate of soda, sodium lauryl sulphate, magnesium chloride, gac and zeyssatite successively, and under 55 ℃～60 ℃ temperature, be incubated 10 minutes～30 minutes;
The vitamin G dissolving with hydrochloric acid liquid that (3) in suction filter, will pass through step (2) processing behind the two-layer acidproof cloth of place mat carries out suction filtration or press filtration, and gained filtrating is filtered through the acidproof microporous membrane filters in three roads more successively;
(4) in crystallizer, add deionized water and also use steam heating; To be crystallized jar jar temperature reaches 90 ℃ of membrane filtration liquid that add in the step (3); Crystallizer is warming up to 95 ℃～98 ℃ and keep this temperature and change brilliant; Change steam off valve after brilliant 2～3 hours, the cooling of open cold penstock is treated will change when temperature is reduced to 25 ℃～30 ℃ brilliant liquid and is put into whizzer and separate;
(5) separate to finish the back and wash with deionized water, wash PH to the PH of mother liquor and deionized water identical till, washing back drying 25～30 minutes;
(6) dry, pulverize, sieve;
Wherein: add 0.04 milliliter～0.06 milliliter in ydrogen peroxide 50, zinc sulfate 0.006 gram～0.012 gram, yellow prussiate of soda 0.006 gram～0.012 gram, sodium lauryl sulphate 0.008 gram～0.015 gram, magnesium chloride 0.008 gram～0.015 gram in the every gram vitamin G in the step (2); Gac 0.015 gram～0.020 gram, zeyssatite 0.04 gram～0.08 gram.
The technical scheme of further optimizing as the present invention: add 0.05 milliliter in ydrogen peroxide 50, zinc sulfate 0.008 gram, yellow prussiate of soda 0.008 gram, sodium lauryl sulphate 0.01 gram, magnesium chloride 0.01 gram, gac 0.018 gram, zeyssatite 0.06 gram in the every gram vitamin G in the said step (2).
Filtrating needs the acidproof microporous membrane in three roads of process to be followed successively by 1.0 μ films, 0.45 μ film and 0.1 μ film in the said step (3).
Add deionized water in the said step (4), make the concentration of vitamin G reach 10～15 grams per liters.
The technical scheme of further optimizing as the present invention: add deionized water in the said step (4), make the concentration of vitamin G reach 12 grams per liters.
The invention has the advantages that: the production technique that the present invention relates to the bullion of vitamin G (Wei ShengsuB2) is carried out purification refine; The present invention has advantages such as purifying process is simple, easy and simple to handle, with low cost, purifying rear impurity content is low, and vitamin G content can be purified to more than 98%.
Embodiment
Below in conjunction with specific embodiment the present invention is further specified:
Embodiment 1: in temperature be under 55 ℃～60 ℃ the agitation condition with 100 gram vitamin G dissolving crude products in 250 milliliters of the technical hydrochloric acids of concentration >=30%; In vitamin G dissolving with hydrochloric acid liquid, add 5 milliliters in ydrogen peroxide 50, zinc sulfate 0.8 gram, yellow prussiate of soda 0,8 grams, sodium lauryl sulphate 1 gram, magnesium chloride 1 gram, gac 1.8 grams, zeyssatite 6 grams successively.And under 55 ℃～60 ℃ temperature, be incubated 30 minutes; In suction filter, behind the two-layer acidproof cloth of place mat vitamin G dissolving with hydrochloric acid liquid is carried out suction filtration or press filtration, gained filtrating is filtered through the acidproof microporous membrane filters in three roads that is followed successively by 1.0 μ films, 0.45 μ film and 0.1 μ film successively; The adding deionized water makes the concentration of vitamin G reach 12 grams per liters and uses steam heating in crystallizer; To be crystallized jar jar temperature reaches 90 ℃ and adds membrane filtration liquid; Crystallizer is warming up to 95 ℃～98 ℃ and keep this temperature and change brilliant; Change steam off valve after brilliant 2.5 hours, the cooling of open cold penstock is treated will change when temperature is reduced to 25 ℃～30 ℃ brilliant liquid and is put into whizzer and separate; Separate to finish the back and wash with deionized water, wash PH to the PH of mother liquor and deionized water identical till, washing back drying 25 minutes; Dry, pulverize, sieve.
Embodiment 2: in temperature be under 55 ℃～60 ℃ the agitation condition with 100 gram vitamin G dissolving crude products in 300 milliliters of the technical hydrochloric acids of concentration >=30%; In vitamin G dissolving with hydrochloric acid liquid, add 4 milliliters in ydrogen peroxide 50, zinc sulfate 0.6 gram, yellow prussiate of soda 0,6 grams, sodium lauryl sulphate 0.8 gram, magnesium chloride 0.8 gram, gac 1.5 grams, zeyssatite 4 grams successively.And under 55 ℃～60 ℃ temperature, be incubated 20 minutes; In suction filter, behind the two-layer acidproof cloth of place mat vitamin G dissolving with hydrochloric acid liquid is carried out suction filtration or press filtration, gained filtrating is filtered through the acidproof microporous membrane filters in three roads that is followed successively by 1.0 μ films, 0.45 μ film and 0.1 μ film successively; The adding deionized water makes the concentration of vitamin G reach 10 grams per liters and uses steam heating in crystallizer; To be crystallized jar jar temperature reaches 90 ℃ and adds membrane filtration liquid; Crystallizer is warming up to 95 ℃～98 ℃ and keep this temperature and change brilliant; Change steam off valve after brilliant 3 hours, the cooling of open cold penstock is treated will change when temperature is reduced to 30 ℃ brilliant liquid and is put into whizzer and separate; Separate to finish the back and wash with deionized water, wash PH to the PH of mother liquor and deionized water identical till, washing back drying 30 minutes; Dry, pulverize, sieve.
Present embodiment only is the preferred embodiments of the invention in sum; Unintelligible is qualification to protection domain of the present invention; For technical work personnel present embodiment is done according to the present invention the adjustment that does not exceed technical scheme of the present invention and the change in this field, should think and drop in protection scope of the present invention.
Claims (5)
1. vitamin G process for purification refine is characterized in that: comprise following process step:
(1) temperature be under 55 ℃～60 ℃ the agitation condition with every gram vitamin G dissolving crude product in 2.5 milliliters～3.0 milliliters of the technical hydrochloric acids of concentration >=30%;
(2) in vitamin G dissolving with hydrochloric acid liquid, add ydrogen peroxide 50, zinc sulfate, yellow prussiate of soda, sodium lauryl sulphate, magnesium chloride, gac and zeyssatite successively, and under 55 ℃～60 ℃ temperature, be incubated 10 minutes～30 minutes;
The vitamin G dissolving with hydrochloric acid liquid that (3) in suction filter, will pass through step (2) processing behind the two-layer acidproof cloth of place mat carries out suction filtration or press filtration, and gained filtrating is filtered through the acidproof microporous membrane filters in three roads successively;
(4) in crystallizer, add deionized water and also use steam heating; To be crystallized jar jar temperature reaches 90 ℃ of membrane filtration liquid that add in the step (3); Crystallizer is warming up to 95 ℃～98 ℃ and keep this temperature and change brilliant; Change steam off valve after brilliant 2～3 hours, the cooling of open cold penstock is treated will change when temperature is reduced to 25 ℃～30 ℃ brilliant liquid and is put into whizzer and separate;
(5) separate to finish the back and wash with deionized water, wash pH to the pH of mother liquor and deionized water identical till, washing back drying 25～30 minutes;
(6) dry, pulverize, sieve;
Wherein: add 0.04 milliliter～0.06 milliliter in ydrogen peroxide 50, zinc sulfate 0.006 gram～0.012 gram, yellow prussiate of soda 0.006 gram～0.012 gram, sodium lauryl sulphate 0.008 gram～0.015 gram, magnesium chloride 0.008 gram～0.015 gram in the every gram vitamin G in the step (2); Gac 0.015 gram～0.020 gram, zeyssatite 0.04 gram～0.08 gram.
2. vitamin G process for purification refine according to claim 1 is characterized in that: add 0.05 milliliter in ydrogen peroxide 50, zinc sulfate 0.008 gram, yellow prussiate of soda 0.008 gram, sodium lauryl sulphate 0.01 gram, magnesium chloride 0.01 gram, gac 0.018 gram, zeyssatite 0.06 gram in the every gram vitamin G in the said step (2).
3. vitamin G process for purification refine according to claim 1 is characterized in that: filtrating needs the acidproof microporous membrane in three roads of process to be followed successively by 1.0 μ films, 0.45 μ film and 0.1 μ film in the said step (3).
4. vitamin G process for purification refine according to claim 1 is characterized in that: add deionized water in the said step (4), make the concentration of vitamin G reach 10～15 grams per liters.
5. vitamin G process for purification refine according to claim 1 is characterized in that: add deionized water in the said step (4), make the concentration of vitamin G reach 12 grams per liters.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102930007A CN101941974B (en) | 2010-09-15 | 2010-09-15 | Purification method of riboflavin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102930007A CN101941974B (en) | 2010-09-15 | 2010-09-15 | Purification method of riboflavin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101941974A CN101941974A (en) | 2011-01-12 |
| CN101941974B true CN101941974B (en) | 2012-09-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2010102930007A Active CN101941974B (en) | 2010-09-15 | 2010-09-15 | Purification method of riboflavin |
Country Status (1)
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104473269A (en) * | 2014-11-21 | 2015-04-01 | 安徽农业大学 | Method for improving light stability of riboflavin in aqueous solution and application thereof |
| CN109851619B (en) * | 2019-02-02 | 2021-04-23 | 赤峰制药股份有限公司 | Riboflavin purification process |
| CN110272424A (en) * | 2019-06-29 | 2019-09-24 | 赤峰制药股份有限公司 | A method of extracting riboflavin from Lactochrome fermentation liquor |
| CN111072664B (en) * | 2019-12-30 | 2021-03-23 | 北京和合医学诊断技术股份有限公司 | Method for purifying vitamin B2 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1146455A (en) * | 1995-03-03 | 1997-04-02 | 弗·哈夫曼-拉罗切有限公司 | Purification for riboflavin |
| CN1687069A (en) * | 2005-04-27 | 2005-10-26 | 浙江钱江生物化学股份有限公司 | Method for extracting vitamine B2 |
| CN1765897A (en) * | 2004-10-27 | 2006-05-03 | 上海凯赛生物技术研发中心有限公司 | Lactochrome fermentation liquor extraction process |
-
2010
- 2010-09-15 CN CN2010102930007A patent/CN101941974B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1146455A (en) * | 1995-03-03 | 1997-04-02 | 弗·哈夫曼-拉罗切有限公司 | Purification for riboflavin |
| CN1765897A (en) * | 2004-10-27 | 2006-05-03 | 上海凯赛生物技术研发中心有限公司 | Lactochrome fermentation liquor extraction process |
| CN1687069A (en) * | 2005-04-27 | 2005-10-26 | 浙江钱江生物化学股份有限公司 | Method for extracting vitamine B2 |
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| CN101941974A (en) | 2011-01-12 |
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Denomination of invention: Purification of riboflavin Effective date of registration: 20210223 Granted publication date: 20120926 Pledgee: Agricultural Bank of China Limited Chifeng Baima sub branch Pledgor: CHIFENG PHARMACEUTICAL Co.,Ltd. Registration number: Y2021150000018 |
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Denomination of invention: Purification and refining method of riboflavin Granted publication date: 20120926 Pledgee: Agricultural Bank of China Limited Chifeng Baima sub branch Pledgor: CHIFENG PHARMACEUTICAL Co.,Ltd. Registration number: Y2024150000003 |