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Medicinal folic acid purifying method

A purification method, technology of folic acid, applied in the direction of organic chemistry, etc.

Active Publication Date: 2014-10-15
JINAN KANGHE MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009]Patents US2694710 and US2634271 respectively introduced the method of purifying folic acid. The samples obtained by the purification method introduced by the above-mentioned patents have been tested and can no longer meet the current quality standards of folic acid used in medicine
However, other existing methods are either unable to realize industrialization or have high purification costs. Therefore, it is very urgent to find an economical, practical and easy-to-operate refining method.

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0028] Slowly add 470 ml of 40% sulfuric acid solution to 50 g of crude folic acid (tested by the Pharmacopoeia HPLC method, the purity of folic acid is 91.1%, and the content of pteroic acid is 2.8%), control the temperature at about 55°C, and stir until the solid is completely dissolved, and stir for half an hour. Slowly add 1.6L of purified water dropwise, temperature control ≤ 60°C, stirring speed 750 rpm, solid precipitates, cool down, filter with suction, wash with a small amount of ethanol, and dry. Add the refined product into purified water, heat to 90-100°C, add 5.8g of sodium hydroxide in batches, adjust pH=11.9 until the solid is completely dissolved, add 2.5g of activated carbon, heat to boiling for 45 minutes, and filter while hot. Slowly add 6M hydrochloric acid solution dropwise to the mother liquor while it is hot, adjust the pH=2.9, cool down and stir to crystallize, filter with suction, wash with sodium bicarbonate solution, purified water and a small amount ...

Embodiment 2

[0030] Add 50g of crude folic acid (tested by Pharmacopoeia HPLC method, folic acid purity 91.1%, pteroic acid content 2.8%) into 1.5L of purified water, heat to 90-100°C, add 8.3g of solid sodium hydroxide in batches, adjust pH=11.8 , when the solid is completely dissolved, add 2.5g of activated carbon, heat to boiling for 45 min, and filter while hot. Slowly add the mother liquor while hot concentrated hydrochloric acid solution , adjust the pH=2.2, cool down, stir and crystallize, and filter and dry. Slowly add 450ml of 40% sulfuric acid solution into the primary refined folic acid, control the temperature at about 55°C, stir until the solid is completely dissolved, and stir for half an hour. Slowly add 1.5 L of purified water dropwise, temperature control ≤ 60°C, stirring speed 750 rpm, solid precipitates, cool down, filter with suction, wash with a small amount of ethanol, and dry. Add the secondary refined product into purified water, heat to 90-100°C, add 6.0g of sod...

Embodiment 3

[0032]Add 50 g of crude folic acid (tested by Pharmacopoeia HPLC method, folic acid purity 91.1%, pteroic acid content 2.8%) into 1.5 L of purified water, heat to 90-100 °C, add 8.5 g of solid sodium hydroxide in batches, adjust pH=12.1, After the solid is completely dissolved, add 2.5 g of activated carbon, heat to boiling for 45 min, and filter while hot. Slowly add 6M hydrochloric acid solution dropwise to the mother liquor while it is hot, adjust the pH=3.1, cool down, stir and crystallize, and filter and dry. Will 50% sulfuric acid solution Slowly add 440ml into the primary refined folic acid, control the temperature at about 55°C, stir until the solid is completely dissolved, and stir for half an hour. Slowly add 1.5 L of purified water dropwise, temperature control ≤ 60°C, stirring speed 750 rpm, solid precipitates, cool down, filter with suction, wash with a small amount of ethanol, and dry. Add the secondary refined product into purified water, heat to 90-100°C, ad...

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Abstract

The invention provides a medicinal folic acid purifying method. According to the method, an acid-alkali method is systematically utilized for purifying folic acid crude products, folic acid finished products meeting pharmacopoeia standards can be prepared repetitively, folic acid purity is above 99%, and the content of pteroic acid impurities in refined folic acid is below 0.1%. The medicinal folic acid purifying method has the advantages that on one hand, the medicinal folic acid purifying method is used for refining the folic acid crude products aiming at the pteroic acid impurities difficult to remove, and is low in cost, simple and convenient to operate and easy to boost; on the other hand, purity and production efficiency of the folic acid can be improved effectively, and development and application in scale production are benefited.

Description

technical field [0001] The invention belongs to the field of compound preparation, and in particular relates to a method for purifying medicinal folic acid. technical background [0002] Folic acid is a B vitamin widely found in green vegetables and fruits. In 1941, American scholar Mitchell and others discovered this compound with anti-anemia effect in spinach. Because this compound mainly comes from the leaves of the plant, it was named folic acid. In 1945, Angier et al. synthesized folic acid and completed the determination of its structure. [0003] Folic acid is known as vitamin B 9 Or Bc, whose chemical name is pteroylglutamic acid. The structure of folic acid contains pteridine, p-aminobenzoic acid and glutamic acid structures. The finished product of folic acid is an orange-yellow crystal, which can be decomposed when heated to 250°C. Folic acid is a kind of organic substance necessary to maintain the normal life activities of living organisms. After being absor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D475/04
CPCC07D475/04
Inventor 张颖刘真豪刘鹏郑良文朱玉正高国锐王学斌刘元鑫
Owner JINAN KANGHE MEDICAL TECH
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