Method for separating adenosine cyclic 3',5'-(hydrogen phosphate) from catalytic liquid through macroporous adsorptive resins
A cyclic adenosine monophosphate, pore adsorption technology, applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve incomplete elution of cyclic adenosine monophosphate, poor adsorption selectivity, high concentration of pigments and impurities, etc. problems, achieve the effect of shortening the process cycle, shortening the time and improving the purity
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Embodiment 1
[0035] The small test of embodiment 1 cyclic adenosine monophosphate separation
[0036] Take 50mL of cyclic adenosine monophosphate catalytic solution, in which the concentration of cAMP is about 5.0g / L, ATP 7g / L, pyruvate 8g / L, MgCl 2 5.6g / L, potassium dihydrogen phosphate 4g / L. The pH of the solution was first adjusted to 2.8, and then centrifuged at 4000 rpm for 15 minutes to collect 35 mL of supernatant. Then the column separation was performed on a glass chromatography column equipped with HP-20 resin, and pure water was used for elution. The loading capacity of the resin in the chromatography column is 235g, the porosity of the bed is 0.33, and the total volume of the bed is about 350mL. The flow rates of loading and elution are both 1BV / h. Then the eluate is collected in sections, and the concentration of cyclic adenosine monophosphate, ATP, and magnesium ions is measured, and the concentration of each component in the effluent is as described in the patent figur...
Embodiment 2
[0037] Embodiment 2 Scale-up of separation of cyclic adenosine monophosphate
[0038] Take 1L of cyclic adenosine monophosphate catalytic solution, in which the concentration of cAMP is about 6g / L, ATP 3g / L, pyruvate 7g / L, MgCl 2 6g / L, potassium dihydrogen phosphate 2g / L, first adjust the pH of the solution to 3.0, then centrifuge at 4000 rpm for 15 minutes, and collect 920mL of supernatant. Then the column separation was performed on a glass chromatography column equipped with HP-20 resin, and pure water was used for elution. The loading capacity of the resin in the chromatography column is 2000g, the porosity of the bed is 0.33, and the total volume of the bed is about 3L. The flow rates of loading and elution are both 1BV / h. Then the eluate was collected in sections, and the concentrations of cyclic adenosine monophosphate, ATP and magnesium ions were determined. The cAMP eluate collected has a volume of 9200 mL, a concentration of 0.6 g / L, a purity of 96%, and a yield of...
Embodiment 3
[0039] Chromatographic separation and crystallization of embodiment 3 cyclic adenosine monophosphate
[0040] Take 3L cyclic adenosine monophosphate catalytic solution, wherein the concentration of cAMP is about 6.7g / L, ATP 2g / L, pyruvate (6g / L, MgCl 2 5.2g / L, potassium dihydrogen phosphate 3g / L, first adjust the pH of the solution to 2.9, then centrifuge at 5000 rpm for 12 minutes, and collect 2790mL of supernatant. Then, it was separated on a glass chromatography column equipped with HP-20 resin, and eluted with pure water. The loading capacity of the resin in the chromatography column is 6000g, the porosity of the bed is 0.33, and the total volume of the bed is about 9L. The flow rates of loading and elution are both 1BV / h. Then the eluate was collected in sections, and the concentrations of cyclic adenosine monophosphate, ATP and magnesium ions were determined. The cAMP eluate collected has a volume of 28.5 L, a concentration of 0.59 g / L, a purity of 97.2%, and a yield...
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