Preparation method of cobamamide crude product
A technology for adenosylcobalamin and crude product, which is applied in the field of preparation of crude adenosylcobalamin, can solve the problems of generating a lot of waste water, affecting the continuity of operations, and many times of dismantling and washing.
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Embodiment 1
[0027] Take 15kg of adenosylcobalamin mycelium powder (containing 0.029kg of adenosylcobalamin), put it into a solvent extraction tank, and add acetone to compound Solvent (acetone (v): isopropanol (v): water (v) = 3.5:1.5:5.5), control the stirring speed at 60rpm, and carry out leaching at room temperature. After leaching for 3 hours, filter in a centrifuge and collect the filter residue. Carry out the second leaching as before, combine the two extracts, and concentrate under reduced pressure with a thin-film evaporator to obtain adenosylcobalamin concentrated solution I 39L (potency 718 μg / ml), with a yield of 96.6%.
[0028] Put the above adenosylcobalamin concentrated solution I into the macroporous resin adsorption column, and then use 30% (v / v), 40% (v / v), 50% (v / v) acetone aqueous solution to analyze in sequence, and collect the analysis solution , concentrated under reduced pressure with a thin-film evaporator to obtain adenosylcobalamin concentrate II 75L (titer 358μg...
Embodiment 2
[0032] Take 15kg of adenosylcobalamin mycelium powder (containing 0.029kg of adenosylcobalamin), put it into a solvent extraction tank, and add acetone to compound Solvent (acetone (v): isopropanol (v): water (v) = 4.0:1.7:6.0), control the stirring speed at 60rpm, carry out leaching at room temperature, after leaching for 3 hours, filter in a centrifuge, collect the filter residue, Carry out the second leaching as before, combine the two extracts, concentrate under reduced pressure to obtain 43 L of extract concentrate, the concentration of the concentrate is 660 μg / ml, and the yield is 97.9%.
[0033] Put the above adenosylcobalamin concentrated solution I into the macroporous resin adsorption column, and then use 30% (v / v), 40% (v / v), 50% (v / v) acetone aqueous solution to analyze in sequence, and collect the analysis solution , concentrated under reduced pressure with a thin film evaporator to obtain adenosylcobalamin concentrate II 79L (titer 350μg / ml), yield 97.4%.
[00...
Embodiment 3
[0037]Take 15kg of adenosylcobalamin mycelium powder (containing 0.029kg of adenosylcobalamin), put it into a solvent extraction tank, and add acetone to compound Solvent (acetone (v): isopropanol (v): water (v) = 4.5:2.0:6.5), control the stirring speed at 60rpm, carry out leaching at room temperature, after leaching for 3 hours, filter in a centrifuge, collect the filter residue, Carry out the second leaching as before, combine the three leaching liquids, and concentrate under reduced pressure to obtain 45 L of leaching concentrated liquid, the concentration of the concentrated liquid is 630 μg / ml, and the yield is 97.8%.
[0038] Put the above adenosylcobalamin concentrated solution I into the macroporous resin adsorption column, and then use 30% (v / v), 40% (v / v), 50% (v / v) acetone aqueous solution to analyze in sequence, and collect the analysis solution , concentrated under reduced pressure with a thin-film evaporator to obtain adenosylcobalamin concentrate II 81L (titer ...
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