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The synthetic method of sodium bisulfite andrographolide

A technology of sodium bisulfite and andrographolide, applied in the field of medicine, can solve problems such as environmental pollution, high impurity content, unstable product quality, etc., and achieve the effect of stable product quality and low impurity content

Inactive Publication Date: 2011-12-14
李宏 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Existing methods of producing sodium bisulfite andrographolide mostly adopt chloroform to extract impurities. This method mainly has two deficiencies. The one is that the impurity content is higher in the product, and the product quality is unstable; Chloroform, easy to cause environmental pollution

Method used

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  • The synthetic method of sodium bisulfite andrographolide
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  • The synthetic method of sodium bisulfite andrographolide

Examples

Experimental program
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Effect test

Embodiment 1

[0031] A kind of synthetic method of sodium bisulfite andrographolide, comprises the steps:

[0032] (1) 350 parts by weight of andrographolide being dissolved in 2947 parts by weight of 95% ethanol aqueous solution;

[0033] (2) the sodium bisulfite of 114 parts by weight is dissolved in the water of 650 parts by weight;

[0034] (3) Add the solution prepared in step (2) to the solution prepared in step (1), and react at 60-70°C for 2 hours;

[0035] (4) Ethanol is evaporated at a vacuum degree of 0.099MPa and a temperature of 43°C;

[0036] (5) cooling to 10°C, standing for 10 hours, adding 2 parts by weight of activated carbon to filter;

[0037] (6) Add hydrochloric acid equivalent to sodium bisulfite to the filtrate, cool to 0°C, and crystallize;

[0038] (7) Dissolve the crystals precipitated in step (6) in 1.2 times the water at 60° C. of the crystals, add sodium carbonate to make the pH 5.2, cool to 0° C., and separate out sodium bisulfite andrographolide crystals. ...

Embodiment 2

[0040] A kind of synthetic method of sodium bisulfite andrographolide, comprises the steps:

[0041] (1) 350 parts by weight of andrographolide being dissolved in 2100 parts by weight of ethanol with a weight percent concentration of 100%;

[0042] (2) the sodium bisulfite of 100 parts by weight is dissolved in the water of 700 parts by weight;

[0043] (3) Add the solution prepared in step (2) to the solution prepared in step (1), and react at 40°C-50°C for 6 hours;

[0044] (4) Ethanol is evaporated at a vacuum degree>0.03MPa and a temperature of 85°C;

[0045] (5) cooling to 0 DEG C, standing for 1 hour, adding 1 weight part of activated carbon to filter;

[0046] (6) Add sulfuric acid equivalent to 0.7 times equivalent of sodium bisulfite to the filtrate, cool to -5°C, and crystallize;

[0047] (7) Dissolve the crystals precipitated in step (6) in water at 40°C that is 0.6 times the size of the crystals, add sodium hydroxide to make the pH 4.0, cool to -5°C, and precipi...

Embodiment 3

[0049] A kind of synthetic method of sodium bisulfite andrographolide, comprises the steps:

[0050] (1) 350 parts by weight of andrographolide being dissolved in 4890 parts by weight of ethanol aqueous solution with a concentration of 50% by weight;

[0051] (2) the sodium bisulfite of 200 parts by weight is dissolved in the water of 1000 parts by weight;

[0052] (3) Add the solution prepared in step (2) to the solution prepared in step (1), and react at 85°C-95°C for 0.5 hours;

[0053] (4) Ethanol is evaporated at a vacuum degree of >0.07MPa and a temperature of 60°C;

[0054] (5) be cooled to 30 DEG C, leave standstill for 12 hours, add 8 parts by weight of activated carbon to filter;

[0055] (6) Add nitric acid equivalent to 1.5 times the equivalent of sodium bisulfite in the filtrate, cool to 40°C, and crystallize;

[0056] (7) Dissolve the crystals precipitated in step (6) in 90° C. water 2.2 times larger than the crystals, add sodium bicarbonate to make the pH 6.5...

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Abstract

The invention discloses a synthesis method of sodium bisulfite andrographolide, which comprises the following steps: (1) dissolving andrographolide in ethanol aqueous solution or methanol aqueous solution; (2) dissolving sodium bisulfite in water; 3) Add the solution prepared in step (2) to the solution prepared in step (1), and react at 40-95°C for 0.5-6 hours; (4) Ethanol or methanol is evaporated at a vacuum degree>0.03MPa; (5) cooling, leave standstill, add gac to filter; (6) add acid in the filtrate, cooling, crystallization; (7) the crystallization that step (6) is separated out is dissolved in water, adds sodium carbonate, makes pH be 4.0~ 6.5, cooling, and the crystallization of sodium bisulfite andrographolide is separated out. The sodium bisulfite andrographolide produced by the present invention has low impurity content, stable product quality, and a content of more than 99.8%, ensuring the safety of clinical medication. The present invention is in the preparation process Avoid the use of chloroform, which is good for the environment.

Description

technical field [0001] The invention belongs to the field of medicine, and relates to a method for synthesizing sodium bisulfite andrographolide. Background technique [0002] Sodium bisulfite andrographolide is the raw material of Lianbizhi Injection, which is widely used clinically in diseases such as dysentery, pneumonia, acute tonsillitis, mumps, laryngitis and upper respiratory tract infection caused by bacteria. [0003] Existing methods of producing sodium bisulfite andrographolide mostly adopt chloroform to extract impurities. This method mainly has two deficiencies. The one is that the impurity content is higher in the product, and the product quality is unstable; Chloroform is easy to cause environmental pollution. Contents of the invention [0004] The purpose of the invention is to overcome the deficiencies in the prior art, to provide a low impurity content, stable product quality; a kind of synthetic method of sodium bisulfite andrographolide that does not u...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/58
Inventor 杨浦生李宏岳昌林
Owner 李宏