CN1286837C - Method for extracting vitamine B2 - Google Patents
Method for extracting vitamine B2 Download PDFInfo
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- CN1286837C CN1286837C CN 200510049680 CN200510049680A CN1286837C CN 1286837 C CN1286837 C CN 1286837C CN 200510049680 CN200510049680 CN 200510049680 CN 200510049680 A CN200510049680 A CN 200510049680A CN 1286837 C CN1286837 C CN 1286837C
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Abstract
The present invention relates to a method for extracting vitamin B2 from fermentation liquor of vitamin B2. The existing method for extracting the vitamin B2 by an acid solution method has long process flows, large energy consumption, 60 to 70% of the purity of one-step solution, separation and crystallization, and low yield of multi-purification. The present invention provides a novel method for extracting the vitamin B2, which comprises the steps that calcium chloride, disodium hydrogen phosphate and sodium polyacrylate are added for flocculation, filtered, precipitated by adding hydrogen peroxide, then crystallized and recrystallized. The present invention has the advantages that the present invention breaks through the traditional methods, adopts an alkali solution method and has simple method, short process flow and low operation cost, the extracting process can not cause environmental pollution, with the adoption of the present invention, the extracting yield of the vitamin B2 can reach 85 to 87%, and the purity of the product can reach 98 to 100%.
Description
Technical field
The invention belongs to a kind of chemical extraction technology, particularly relate to a kind of from vitamins B
2The broth extraction vitamins B
2Method.
Background technology
Vitamins B
2Be that animal metabolism is essential and self can not the synthetic organism.Vitamins B
2Main it can be improved food conversion ratio as additive for farm animal feed, promotes growth of animal, improves the fecundity of animal and the ability of opposing severe environment, and has plurality of health care functions and therapeutic action such as anti-oxidant preventing tumor.Document and textbook are all talked about vitamins B
2It is easily destroyed to meet alkali, so to vitamins B
2The research of extracting concentrates on mostly with strong acid dissolving vitamins B
2Method; Also adopt acid pasting to extract vitamins B in the production
2This extracting method technical process is long, energy consumption is big, once dissolves, separation, crystalline purity only 60%～70%, and repeatedly purification yield is lower.Cause the business equipment input many thus, the production cost height, and environmental pollution is big.
Summary of the invention
The objective of the invention is to overcome the deficiency that above-mentioned technology exists, propose a kind of new vitamins B
2Extracting method is to improve vitamins B
2Extract yield, reduce vitamins B
2The leaching process production cost.
The objective of the invention is to realize: a kind of vitamins B by following technical proposal
2Extracting method, it is made up of the following step:
(1) by 1: 1 thin up vitamins B
2Fermented liquid is regulated pH value to 11.8 with liquid caustic soda, makes it dissolving;
(2) adding calcium chloride, Sodium phosphate dibasic and sodium polyacrylate flocculate and filter; Wherein the add-on of calcium chloride is 0.4% of a reduction of feed volume, and the add-on of Sodium phosphate dibasic is 0.4% of a reduction of feed volume, and sodium polyacrylate should be made into 0.5% the aqueous solution earlier and add, and the add-on of 0.5% polyacrylic acid sodium water solution is 2.5% of a reduction of feed volume;
(3) add 0.20%～0.25% hydrogen peroxide in gained filtrate, the blowing air bubbling stirs, and uses salt acid for adjusting pH value to 4.0～4.2 simultaneously, and solid is separated out;
(4) quiescent setting goes supernatant liquid to half, and leftover materials are heated to boiling, and cooling is rapidly filtered again, obtains vitamins B
2Coarse crystallization;
(5) at the gained vitamins B
2Add water in the coarse crystallization, regulate pH value to 11.8, make it dissolving, refilter with liquid caustic soda;
(6) repeating step (3) and step (4) obtain vitamins B
2Recrystallization;
(7) dry, pulverize, sieve.
The add-on of water is 13 times to 15 times of coarse crystallization in described step (5).
The time of blowing air bubbling is 30min～1hr in described step (3); The time of quiescent setting is 2hr in described step (4).
Drying in described step (7) is 60 ℃ of oven dry down, sieves and adopts 80 mesh sieves.
Adopt the HPLC method to analyze and follow the tracks of discovery: vitamins B
2Under suitable alkaline condition, not only solubleness is big, also demonstrates certain stability; Vitamins B
2At pH is that solubleness is the highest in 11.8 the solution, and room temperature was placed 2 days under this pH value, and the rate of descent of tiring is 7.9% only, has certain stability.Therefore, the present invention breaks through convention, adopts alkali solution technique, and method is simple, and flow process is short, and running cost is low; Leaching process " three wastes " is few, environmentally safe.Adopt the present invention, vitamins B
2Extract yield be 85%～87%, product purity can reach 98%～100%.Quality product meets " Chinese veterinary drug allusion quotation " version one ministerial standard in 2000, and its leading indicator is:
Proterties: orange-yellow crystalline powder, little smelly, mildly bitter flavor;
Differentiate:
(1) chemical reaction is positive reaction,
(2) uv-absorbing has maximum absorption at 267nm, 375nm and 444nm place; The ratio of the optical density of 375nm and the optical density of 267nm is 0.31～0.33; The ratio of the optical density of 444nm and the optical density of 267nm is 0.36～0.39;
Check:
(1) potential of hydrogen: up to specification,
(2) 6,7-dimethylisoalloxazine: be not more than 0.016,
(3) weight loss on drying: be not more than 1.0%,
(4) vehement burning residue: be not more than 0.2%;
Assay: press dry product and calculate, contain (C
17H
20N
4O
6) be 98.0%～102.0%.
Embodiment
Embodiment 1:
Get the 1000ml vitamins B
2Fermented liquid (18212 μ g/ml tire) adds the dilution of 1000ml water, and the liquid caustic soda with 30% is regulated pH value to 11.8, stirs 30min; Add calcium chloride 8g, Sodium phosphate dibasic 8g and 5% sodium polyacrylate solution 50ml and flocculate, filter then; Gained filtrate adds 2.5mlH
2O
2, regulate pH to 4.2 with hydrochloric acid, and the blowing air bubbling stirs 30min; Static 2hr outwells half with supernatant liquid, and residue feed liquid heated and boiled 15min is cooled to room temperature, filters filter cake and cleans with pure water, and crude product 18.5g must wet; Use the 250ml water dissolution, regulate pH to 11.8 with 30% liquid caustic soda again, make material dissolution, filter; Filtrate adds H again
2O
22.5ml, and regulate pH to 4.2 with hydrochloric acid, the blowing air bubbling stirs 30min; Static 2hr, heated and boiled 15min is cooled to room temperature, filters, and gets finished product; 60 ℃ of oven dry are pulverized, and cross 80 mesh sieves, and measuring content is 99.8%, and yield is 86.5%.
Embodiment 2:
Get 1000ml fermented liquid (17924 μ g/ml tire), add the dilution of 1000ml water, the liquid caustic soda with 30% is regulated pH value to 11.8, stirs 30min; Add calcium chloride 8g, Sodium phosphate dibasic 8g and 5% sodium polyacrylate solution 50ml and flocculate, filter then; Gained filtrate adds 2.0mlH
2O
2, regulate pH to 4.0 and blowing air bubbling stirring 1hr with hydrochloric acid; Static 2hr outwells half with supernatant liquid, and residue feed liquid heated and boiled 15min is cooled to room temperature, filters, and crude product 17.5g must wet; Use the 250ml water dissolution again, the liquid caustic soda with 30% is regulated pH to 11.8, makes material dissolution, filters; Filtrate adds H again
2O
22.0ml and regulate pH to 4.0 with hydrochloric acid, the blowing air bubbling stirs 1hr; Static 2hr, heated and boiled 15min is cooled to room temperature, filters, and gets finished product; 60 ℃ of oven dry are pulverized, and cross 80 mesh sieves, and measuring content is 99.3%, and yield is 85.2%.
Embodiment 3:
Get 1000ml fermented liquid (18122 μ g/ml tire), add the dilution of 1000ml water, the liquid caustic soda with 30% is regulated pH value to 11.8, stirs 30min; Add calcium chloride 8g, Sodium phosphate dibasic 8g and 5% sodium polyacrylate solution 50ml and flocculate, filter then; Gained filtrate adds 2.2mlH
2O
2, regulate pH to 4.1 and blowing air bubbling stirring 40min with hydrochloric acid; Static 2hr outwells half with supernatant liquid, and residue feed liquid heated and boiled 15min is cooled to room temperature, filters, and crude product 17.7g must wet; Use the 230ml water dissolution again, the liquid caustic soda with 30% is regulated pH to 11.8, makes material dissolution, filters; Filtrate adds H again
2O
22.2ml and regulate pH to 4.0 with hydrochloric acid, the blowing air bubbling stirs 1hr; Static 2hr, heated and boiled 15min is cooled to room temperature, filters, and gets finished product; 60 ℃ of oven dry are pulverized, and cross 80 mesh sieves, and measuring content is 98.8%, and yield is 85.0%.
Embodiment 4:
Get 1000ml fermented liquid (17996 μ g/ml tire), add the dilution of 1000ml water, the liquid caustic soda with 30% is regulated pH value to 11.8, stirs 30min; Add calcium chloride 8g, Sodium phosphate dibasic 8g and 5% sodium polyacrylate solution 50ml and flocculate, filter then; Gained filtrate adds 2.4mlH
2O
2, regulate pH to 4.0 and blowing air bubbling stirring 1hr with hydrochloric acid; Static 2hr outwells half with supernatant liquid, and residue feed liquid heated and boiled 15min is cooled to room temperature, filters, and crude product 17.6g must wet; Use the 264ml water dissolution again, the liquid caustic soda with 30% is regulated pH to 11.8, makes material dissolution, filters; Filtrate adds H again
2O
22.4ml and regulate pH to 4.0 with hydrochloric acid, the blowing air bubbling stirs 1hr; Static 2hr, heated and boiled 15min is cooled to room temperature, filters, and gets finished product; 60 ℃ of oven dry are pulverized, and cross 80 mesh sieves, and measuring content is 99.0%, and yield is 85.1%.
Claims (5)
1. vitamins B
2Extracting method is characterized in that it is made up of the following step:
(1) by 1: 1 thin up vitamins B
2Fermented liquid is regulated pH value to 11.8 with liquid caustic soda, makes it dissolving;
(2) adding calcium chloride, Sodium phosphate dibasic and sodium polyacrylate flocculate and filter; Wherein the add-on of calcium chloride is 0.4% of a reduction of feed volume, and the add-on of Sodium phosphate dibasic is 0.4% of a reduction of feed volume, and sodium polyacrylate should be made into 0.5% the aqueous solution earlier and add, and the add-on of 0.5% polyacrylic acid sodium water solution is 2.5% of a reduction of feed volume;
(3) add 0.20%～0.25% hydrogen peroxide in gained filtrate, the blowing air bubbling stirs, and uses salt acid for adjusting pH value to 4.0～4.2 simultaneously, and solid is separated out;
(4) quiescent setting goes supernatant liquid to half, and leftover materials are heated to boiling, and cooling is rapidly filtered again, obtains vitamins B
2Coarse crystallization;
(5) at the gained vitamins B
2Add water in the coarse crystallization, regulate pH value to 11.8, make it dissolving, refilter with liquid caustic soda;
(6) repeating step (3) and step (4) obtain vitamins B
2Recrystallization;
(7) dry, pulverize, sieve.
2. vitamins B according to claim 1
2Extracting method, the add-on that it is characterized in that water in described step (5) are 13 times to 15 times of coarse crystallization.
3. vitamins B according to claim 1 and 2
2Extracting method, the time that it is characterized in that blowing air bubbling in described step (3) is 30min～1hr; The time of quiescent setting is 2hr in described step (4).
4. vitamins B according to claim 1 and 2
2Extracting method is characterized in that the drying in described step (7) is 60 ℃ of oven dry down, sieves and adopts 80 mesh sieves.
5. vitamins B according to claim 3
2Extracting method is characterized in that the drying in described step (7) is 60 ℃ of oven dry down, sieves and adopts 80 mesh sieves.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510049680 CN1286837C (en) | 2005-04-27 | 2005-04-27 | Method for extracting vitamine B2 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510049680 CN1286837C (en) | 2005-04-27 | 2005-04-27 | Method for extracting vitamine B2 |
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| Publication Number | Publication Date |
|---|---|
| CN1687069A CN1687069A (en) | 2005-10-26 |
| CN1286837C true CN1286837C (en) | 2006-11-29 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200510049680 Active CN1286837C (en) | 2005-04-27 | 2005-04-27 | Method for extracting vitamine B2 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101941974B (en) * | 2010-09-15 | 2012-09-26 | 赤峰制药股份有限公司 | Purification method of riboflavin |
| CN103664848B (en) * | 2012-09-13 | 2016-03-23 | 北大方正集团有限公司 | A kind of extracting method of mycophenolic acid |
| CN109134468A (en) * | 2018-07-28 | 2019-01-04 | 广济药业（孟州）有限公司 | Improve bacillus subtilis vitamin B2The method of yield |
| CN110283175A (en) * | 2019-06-29 | 2019-09-27 | 赤峰制药股份有限公司 | A kind of preparation process of high-purity riboflavin |
| CN111690706B (en) * | 2020-06-10 | 2023-06-30 | 浙江钱江生物化学股份有限公司 | Gibberellin A produced by fermentation of riboflavin waste liquid 3 Is a method of (2) |
| CN112125907B (en) * | 2020-09-15 | 2023-05-19 | 宁夏金维制药股份有限公司 | Vitamin B 2 Extraction method |
| CN113667149A (en) * | 2021-06-28 | 2021-11-19 | 山东安华生物医药股份有限公司 | Preparation method of cross-linked hyaluronic acid and tremella polysaccharide |
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