Preparation method of vitamin B12 crude product

A B12 and vitamin technology, applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of easy contamination of centrifuges, affecting continuous operation, and high safety risks.

Active Publication Date: 2020-10-23
NINGXIA KINGVIT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the centrifuge is easy to pollute, it needs to be disassembled and washed many times, which affects the continuous operation, and produces a lot of waste water, which in

Method used

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  • Preparation method of vitamin B12 crude product
  • Preparation method of vitamin B12 crude product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Put 180kg of the above filter residue (potency 560μg / g) into the solvent extraction tank, and add 630L of acetone composite solvent (acetone (V): iso Propanol (V): water (V) = 5.5:1.5:5.5), control the stirring speed at 60rpm, and carry out leaching at room temperature. After leaching for 3 hours, enter the plate frame for filtration, collect the filter residue, and carry out the second leaching as before. , combined the two extracts, and concentrated under reduced pressure to obtain 554 L of extract concentrate (titer 165 μg / ml).

[0031] Combine the extract and filtrate to 1251L (potency 180μg / ml), the volume of the mixed solution is 1805L (potency 175μg / ml), and the yield is 96.9%.

[0032] Put the above mixed solution into a macroporous resin adsorption column, analyze with 30% (v / v), 40% (v / v), and 50% (v / v) acetone aqueous solution in sequence, collect the analysis solution, concentrate under reduced pressure, and obtain adenoid The volume of the concentrated sol...

Embodiment 2

[0037] Put 180kg of the above filter residue (potency 560μg / g) into the solvent extraction tank, and add 720L of acetone composite solvent (acetone (V): iso Propanol (V): water (V) = 6.5:2.5:6.5), control the stirring speed at 60rpm, carry out leaching at room temperature, after leaching for 6 hours, enter the plate frame for filtration, collect the filter residue, and carry out the second leaching as before , combined the two extracts, concentrated under reduced pressure to obtain 604L of extract concentrate (potency 146μg / ml), combined filtrate 1251L (potency 180μg / ml), and mixed solution volume 1855L (potency 169μg / ml). The rate is 96.1%.

[0038]Put the above mixed solution into a macroporous resin adsorption column, analyze with 30% (v / v), 40% (v / v), and 50% (v / v) acetone aqueous solution in sequence, collect the analysis solution, concentrate under reduced pressure, and obtain adenoid Glycobalamin analytical concentrate volume 420L (titer 722μg / ml), yield 96.8%.

[003...

Embodiment 3

[0043] Put 180kg of the above filter residue (potency 560μg / g) into the solvent extraction tank, and add 810L of acetone composite solvent (acetone (v):iso Propanol (v): water (V) = 6.0:2.0:6.0), control the stirring speed at 60rpm, carry out leaching at room temperature, after leaching for 5 hours, enter the plate frame for filtration, collect the filter residue, and carry out the second leaching as before , combined the two extracts, concentrated under reduced pressure to obtain 694L of extract concentrate (potency 135μg / ml), combined filtrate 1251L (potency 180μg / ml), and mixed solution volume 1945L (potency 164μg / ml). The rate is 98.1%.

[0044] Put the above mixed solution into a macroporous resin adsorption column, analyze with 30% (v / v), 40% (v / v), and 50% (v / v) acetone aqueous solution in sequence, collect the analysis solution, concentrate under reduced pressure, and obtain adenoid Glycobalamin analytical concentrate volume 470L (titer 663μg / ml), yield 97.8%.

[004...

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Abstract

The invention relates to a preparation method of a vitamin B12 crude product. A process comprises the following steps: acidifying and hydrolyzing pseudomonas denitrificans, carrying out flocculent precipitation and filtering, and respectively collecting filter residues and filtrate; extracting the filter residues with an acetone composite solvent, mixing the extracted filter residues with the filtrate, and then performing macroporous resin adsorption, acetone aqueous solution desorption and vacuum concentration to obtain a concentrated solution; and performing converting with a cyanamide aqueous solution and crystallizing with acetone to obtain the vitamin B12 crude product. According to the method disclosed by the invention, cobamamide in fungus dregs is extracted by adopting a mixed solution consisting of acetone, isopropanol and water, so that the extraction yield can be effectively improved, the production operation coherence is high, and the generated wastewater amount is small; and cyandiamide is used as a transforming agent to replace sodium cyanide and potassium cyanide, VB12 hydrolysis is not easily caused in the transformation process, the transformation yield is good, the toxicity of the cyanamide is low, the safety and environmental protection pressure is reduced, and enterprises can safely and orderly carry out daily production and operation.

Description

technical field [0001] The invention belongs to the technical field of biological fermentation and extraction, in particular to a method for preparing crude vitamin B12. Background technique [0002] Vitamin B12 (VB12), English name Vitamin B12, also known as cobalamin or cyanocobalamin, is a B vitamin composed of cobalt-containing porphyrin compounds, including adenosylcobalamin (deoxyadenosylcobalamin), cyanocobalamin (cyanocobalamin), methylcobalamin (methylcobalamin), hydroxycobalamin (hydroxycobalamin), the trivalent cobalt contained in it is located in the center of the corrin ring plane similar to porphyrin. In the prior art, vitamin B12 generally specifically refers to cyanocobalamin, and its molecule features a complex formed by cobalt atoms and cyano groups. [0003] Vitamin B12 is the largest and most complex vitamin molecule discovered so far, and it is also the only vitamin containing metal ions; plants do not contain VB12 and cannot manufacture VB12. Liver is...

Claims

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Application Information

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IPC IPC(8): C07H23/00C07H1/00C07H1/06
CPCC07H23/00C07H1/00C07H1/06
Inventor 户鹏东裴立忠高宏伟沈毅马琼
Owner NINGXIA KINGVIT PHARMA
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