A kind of preparation method and application of pteridine folic acid
A technology of pteridine folic acid and glutamic acid, applied in the field of preparation of pteridine folic acid, can solve the problems such as the production mechanism and control method of finished folic acid products that are not deeply studied, and achieve the effect of improving the quality control level of folic acid
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Embodiment 1
[0043] (1) Synthesis of pteridine folic acid crude product
[0044] P-aminobenzoyl glutamic acid, triaminopyrimidine sulfate, trichloroacetone are dissolved in water, wherein based on mass ratio, p-aminobenzoyl glutamic acid: triaminopyrimidine sulfate: trichloroacetone: water = 1:2:3:100, control the pH of the reaction solution to 1, heat to 80°C, keep warm for 5 hours, cool down to 20°C, filter, adjust the pH of the filtrate to 5 with NaOH, and filter to obtain a crude product with a purity of 26.23%;
[0045] (2) Purification of pteridine folic acid
[0046] The crude product was dissolved with ammonia water, filtered, and the filtrate was put into semi-preparative chromatography, 10ml each time, the effluent was collected, combined, concentrated under reduced pressure, and the concentrated solution was diluted 2 times with purified water, then into semi-preparative chromatography, washed with 10% methanol by mass fraction out, collect the effluent, concentrate and freeze-...
Embodiment 2
[0052] (1) Synthesis of pteridine folic acid crude product
[0053] P-aminobenzoyl glutamic acid, triaminopyrimidine sulfate, trichloroacetone are dissolved in water, wherein based on mass ratio, p-aminobenzoyl glutamic acid: triaminopyrimidine sulfate: trichloroacetone: water = 1:3:4:120, control the pH of the reaction solution to 2, heat to 90°C, keep warm for 8 hours, cool down to 30°C, filter, adjust the pH of the filtrate to 3 with NaOH, and filter to obtain a crude product with a purity of 22.51%;
[0054] (2) Purification of pteridine folic acid
[0055] The crude product was dissolved with ammonia water, filtered, and the filtrate was put into semi-preparative chromatography, 10ml each time, the effluent was collected, combined, concentrated under reduced pressure, and the concentrated solution was diluted 2 times with purified water, then into semi-preparative chromatography, washed with 10% methanol by mass fraction out, collect the effluent, concentrate and freeze-...
Embodiment 3
[0058] (1) Synthesis of pteridine folic acid crude product
[0059] P-aminobenzoyl glutamic acid, triaminopyrimidine sulfate, trichloroacetone are dissolved in water, wherein based on mass ratio, p-aminobenzoyl glutamic acid: triaminopyrimidine sulfate: trichloroacetone: water = 1:3:5:150, control the pH of the reaction solution to 2.5, heat to 93°C, keep warm for 9 hours, cool down to 35°C, filter, adjust the pH of the filtrate to 4 with NaOH, and filter to obtain a crude product with a purity of 18.47%;
[0060] (2) Purification of pteridine folic acid
[0061] The crude product was dissolved with ammonia water, filtered, and the filtrate was put into semi-preparative chromatography, 10ml each time, the effluent was collected, combined, concentrated under reduced pressure, and the concentrated solution was diluted 4 times with purified water, then into semi-preparative chromatography, washed with 20% methanol by mass fraction out, collect the effluent, concentrate and freez...
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