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Method for removing solvent residues of diammonium glycyrrhizinate bulk drug

A technology of diammonium glycyrrhizinate and API, applied in steroids, organic chemistry and other directions, can solve problems such as deterioration, difficulty in reaching, darkening in color, etc., and achieve the effects of simple operation, high purity and improved product quality

Active Publication Date: 2019-01-18
河南豫辰药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to experiments, the residual solvent of diammonium glycyrrhizinate raw material drug is difficult to reach the Chinese Pharmacopoeia residual solvent standard of ≤5000ppm by conventional vacuum drying, and the product will become darker and partially deteriorated after long-term vacuum drying

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Put 60 g of crude diammonium glycyrrhizinate and 240 g of 50% ethanol solution into a 500 ml four-necked reaction flask, heat to 65°C to dissolve, add 2.2 g of activated carbon to decolorize for half an hour, and remove the activated carbon by hot filtration. After the filtrate is heated and dissolved, it is cooled to 50°C, added with treated seeds, stirred to cool down for crystallization, a small amount of crystals are precipitated at 47°C, continue to stir, stand at 40°C for crystallization, overnight, and the next day with ice water to cool down to 0~ 5°C, centrifugal filtration to obtain 84.6 g of wet product of diammonium glycyrrhizinate. The obtained wet product was dried under reduced pressure at 55° C. for 6 hours to obtain 49.2 g of primary dry product of diammonium glycyrrhizinate. The obtained primary dry product was placed under the condition of 70% air humidity for 10 hours, and the material weighed 53.2 g after moisture absorption. After the obtained mat...

Embodiment 2

[0021] Put 60 g of crude diammonium glycyrrhizinate and 240 g of 50% ethanol solution into a 500 ml four-necked reaction flask, heat to 65°C to dissolve, add 2.2 g of activated carbon to decolorize for half an hour, and remove the activated carbon by hot filtration. After the filtrate is heated and dissolved, it is cooled to 50°C, added with treated seeds, stirred to cool down for crystallization, a small amount of crystals are precipitated at 47°C, continue to stir, stand at 40°C for crystallization, overnight, and the next day with ice water to cool down to 0~ 5°C, centrifugal filtration to obtain 86.8 g of wet product of diammonium glycyrrhizinate. The obtained wet product was dried under reduced pressure at 55° C. for 7 hours to obtain 48.8 g of a primary dry product of diammonium glycyrrhizinate. The obtained primary dry product was placed under the condition of 80% air humidity for 16 hours, and the material weighed 53.7 g after moisture absorption. The obtained materia...

Embodiment 3

[0023] Put 60 g of crude diammonium glycyrrhizinate and 300 g of 55% ethanol solution into a 500 ml four-necked reaction flask, heat to 65°C to dissolve, add 2.2 g of activated carbon to decolorize for half an hour, and remove the activated carbon by hot filtration. After the filtrate is heated and dissolved, it is cooled to 52°C, added with treated seed crystals, stirred to cool down for crystallization, a small amount of crystals are precipitated at 47°C, continue to stir, stand at 40°C for crystallization, overnight, and the next day with ice water to cool down to 0~ 5°C, centrifugal filtration to obtain 90.1 g of wet product of diammonium glycyrrhizinate. The obtained wet product was dried under reduced pressure at 55° C. for 8 hours to obtain 48.0 g of a primary dry product of diammonium glycyrrhizinate. The obtained primary dry product was placed under the condition of 80% air humidity for 24 hours, and the material weighed 53.5g after moisture absorption. After the obt...

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PUM

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Abstract

The invention discloses a method for removing solvent residues of a diammonium glycyrrhizinate bulk drug. The method comprises the following steps: using a mixing solvent for performing decolorizing re-crystallization on a synthetic crude product of diammonium glycyrrhizinate; centrifugally filtering; drying under reduced pressure; absorbing water and moisture, and then performing suction filtration, and continuing to dry under reduced pressure, thereby acquiring the diammonium glycyrrhizinate bulk drug. Through detection, the residual solvent ethyl alcohol of the acquired diammonium glycyrrhizinate bulk drug is less than or equal to 2000ppm and is far lower than the quality standard (less than or equal to 5000ppm) for residual solvent of diammonium glycyrrhizinate bulk drug in Chinese pharmacopoeia. The diammonium glycyrrhizinate bulk drug is a white granular crystal in larger crystal size and is high in purity and stability.

Description

technical field [0001] The invention belongs to the technical field of production of diammonium glycyrrhizinate bulk medicines, and particularly relates to a method for removing solvent residues of diammonium glycyrrhizinate bulk medicines. Background technique [0002] Diammonium glycyrrhizinate API is the third-generation substitute of the active ingredient of traditional Chinese medicine licorice. At present, after the diammonium glycyrrhizate is synthesized, a method of multiple purifications is used to obtain the diammonium glycyrrhizinate bulk drug, which requires the use of a large amount of solvent, the cost is high, and the obtained product has a high solvent residue. After searching, there is no report on the method of removing solvent residues of diammonium glycyrrhizinate bulk drug. Usually, the removal method of solvent residue is drying and desolvation. Through experiments, it is difficult to achieve the Chinese Pharmacopoeia residual solvent standard of ≤500...

Claims

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Application Information

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IPC IPC(8): C07J63/00
CPCC07J63/008
Inventor 魏利强李闪闪傅收梁永义吴银强罗明石艳彩王心久
Owner 河南豫辰药业股份有限公司
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