Preparation method and application of pteridine folic acid

A technology of pteridine folic acid and sulfate, which is applied in the preparation of test samples, organic chemistry and other directions, can solve the problems such as the production mechanism and control method of finished folic acid products that have not been studied in depth, and achieve the effect of improving the quality control level of folic acid.

Active Publication Date: 2017-11-17
ZHEJIANG SHENGDA BIO PHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods are only from the perspective of how to remove pteridine impurities, and have not studied in dep

Method used

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  • Preparation method and application of pteridine folic acid
  • Preparation method and application of pteridine folic acid
  • Preparation method and application of pteridine folic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (1) Synthesis of crude pteridine folic acid

[0044] Dissolve p-aminobenzoyl glutamic acid, triaminopyrimidine sulfate, and trichloroacetone in water. Based on the 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 it warm for 5 hours, cool 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 is dissolved in ammonia water, filtered, and the filtrate enters the semi-preparative chromatography, 10ml each time, collects the effluent, merges and concentrates under reduced pressure, the concentrate is diluted with purified water twice, and then enters the semi-preparative chromatography, washed with 10% mass fraction of methanol The effluent is collected, concentrated and freeze-dried to obtain pteridine folic acid....

Embodiment 2

[0052] (1) Synthesis of crude pteridine folic acid

[0053] Dissolve p-aminobenzoyl glutamic acid, triaminopyrimidine sulfate, and trichloroacetone in water. Based on the 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 for 8 hours, lower the temperature 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 is dissolved in ammonia water, filtered, and the filtrate enters the semi-preparative chromatography, 10 ml each time, collects the effluent, merges and concentrates under reduced pressure, the concentrate is diluted with purified water twice, and then enters the semi-preparative chromatography, washed with 10% methanol. The effluent is collected, concentrated and freeze-dried to obtain pteridine folic acid, the c...

Embodiment 3

[0058] (1) Synthesis of crude pteridine folic acid

[0059] Dissolve p-aminobenzoyl glutamic acid, triaminopyrimidine sulfate, and trichloroacetone in water. Based on the 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 for 9 hours, lower the temperature 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 is dissolved in ammonia water, filtered, and the filtrate enters the semi-preparative chromatography, 10ml each time, collects the effluent, merges and concentrates under reduced pressure, the concentrate is diluted 4 times with purified water, and then enters the semi-preparative chromatography, washed with 20% methanol by mass fraction The effluent is collected and concentrated and freeze-dried to obtain pteri...

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Abstract

The invention relates to a preparation method and application of pteridine folic acid. The preparation method has the advantages that by using p-aminobenzoyl glutamic acid, triamino pyrimidine sulfate and trichloroacetone as raw materials, and adopting the chemical synthesizing method, the content of crude product of pteridine folic acid is obviously increased; by using preparation chromatography to separate, the pteridine folic acid with purity more than 95% is obtained; the production mechanism and control method of the pteridine folic acid are favorably further studied, and the quality control level of the folic acid is effectively increased.

Description

Technical field [0001] The invention belongs to the field of organic synthesis, and specifically relates to a preparation method of pteridoxidic acid and its application in folic acid quality control. Background technique [0002] 6-pterinylfolic acid [0003] [0004] English name: N,N-bis-[4-[(2-amido-4-oxo-1,4-dihydro-6-terene)methylamino]]benzoyl-L-glutamic acid [0005] Chinese name: N,N-di-(4-((2-amino-4-hydroxy-6-pteridyl)methylamino))benzoyl-L-glutamic acid [0006] Pteridine folic acid is the impurity E of folic acid in EP Pharmacopoeia. [0007] Folic acid, also called vitamin B9, is a water-soluble vitamin that was extracted and purified from spinach leaves by H.K. Mitchell (1941), so it was named folic acid. It has the effect of promoting the maturation of young cells in the bone marrow. The lack of folic acid in humans can cause macrocytic anemia and leukopenia, which is especially important for pregnant women. [0008] Insufficient intake of folic acid can cause a variety...

Claims

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Application Information

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IPC IPC(8): C07D519/00G01N1/28
CPCC07D519/00G01N1/28
Inventor 庞正查张仲景王程鹏许文韬陈优富陈敏陈蒙刘露
Owner ZHEJIANG SHENGDA BIO PHARM
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