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Purification method of puerarin

A purification method and technology of puerarin, applied in the direction of organic chemistry, etc., can solve the problems of not being able to reach the raw materials of injections, limit the application of process routes, and take a long time, and achieve the effects of saving production time, reducing production costs, and reducing the number of crystallization times

Inactive Publication Date: 2018-09-28
REYOUNG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

According to the process route provided by this patent, the extraction test of pueraria root was carried out, and puerarin with a purity greater than 97% can be finally obtained, but according to the external standard method, its content is about 90%, which still cannot meet the requirements of injection raw materials; poly When the amide filler is reused, the column efficiency of the chromatographic column will gradually decrease. In the case of repeated use of polyamide, only 80% of puerarin can be obtained. To obtain puerarin with a content of more than 99%, it is necessary to The puerarin crude product was recrystallized multiple times, and the number of crystallization was as many as 14 times
Due to the long time-consuming crystallization process, the application of this process route is greatly limited

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Concentrate the puerarin eluate to a puerarin concentration of 0.15kg / L, take 2L of the puerarin elution concentrate, add 1kg of 160-mesh neutral alumina, stir and adsorb for 10min, filter, and wash the alumina filter cake with 1L of purified water. Concentrate the eluent at 70°C and 0.05MPa, the concentration of puerarin is 0.15kg / L after concentration, cool down and keep crystallization at 60°C for 20h, filter, add 0.5 times the amount of purified water to the filter cake, heat Dissolve the solid completely at 100°C, then lower the temperature and keep it crystallized at 60°C for 20 hours. After 7 times of crystallization, 121g of puerarin was obtained. The yield of this process is 40.3%, and its content is 99.8%.

Embodiment 2

[0026] Concentrate the puerarin eluate until the puerarin concentration is 0.15kg / L, take 2L of the puerarin elution concentrate, add 0.8kg of 160-mesh neutral alumina, stir and adsorb for 30min, filter, and wash the alumina with 1L of purified water For the filter cake, concentrate the eluent at 90°C and 0.05MPa, the concentration of puerarin is 0.15kg / L after concentration, cool down and keep crystallization at a temperature of 55°C for 12h, filter, add 2 times the amount of solids to the filter cake for purification Water, heated to 80°C to completely dissolve the solid, then lower the temperature and insulate and crystallize at a temperature of 55°C for 12 hours. After 7 times of crystallization, 128g of puerarin was obtained. The yield of this process was 42.7%, and its content was 99.6%.

Embodiment 3

[0028] Concentrate the puerarin eluate until the puerarin concentration is 0.15kg / L, take 2L of the puerarin elution concentrate, add 0.6kg of 200-mesh neutral alumina, stir and adsorb for 10min, filter, and wash the alumina with 1L of purified water For the filter cake, concentrate the eluent at 70°C and 0.06MPa, the concentration of puerarin is 0.15kg / L after concentration, cool down and keep crystallization at a temperature of 50°C for 8 hours, filter, add 6 times the solid amount of purification to the filter cake water, heated to 70°C to completely dissolve the solid, then cooled down and kept at 50°C for 8 hours of crystallization, and crystallized 7 times to obtain 123g of puerarin. The yield of this process was 41.0%, and its content was 99.7%.

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Abstract

The invention relates to a purification method of puerarin and belongs to the technical field of traditional Chinese medicine extraction. The purification method comprises the steps of 1, condensing in vacuum, puerarin elution under the temperature of 60-100 DEG C and vacuum degree of 0.04-0.09 MPa until puerarin concentration is 0.15 kg / L; 2, adding 2 L of the condensed puerarin elution into 0.2-1.0 kg of alumina, and adsorbing by stirring for 10-30 min; 3, filtering, and washing the alumina to obtain puerarin solution; 4, subjecting the puerarin solution of step 3 to septuple crystallizationto obtain puerarin having the content of greater than 99%. The purification method has the advantages that the purification method is scientific and reasonable and is simple and feasible, the purification method of puerarin is greatly simplified, production cost is reduced, and high-purity puerarin is obtained.

Description

technical field [0001] The invention relates to a method for purifying puerarin, which belongs to the technical field of traditional Chinese medicine extraction. Background technique [0002] Puerarin is a single-component flavonoid glycoside extracted from the leguminous plant Pueraria mirifica, which has the functions of promoting blood circulation and removing blood stasis, improving microcirculation, dilating coronary arteries and cerebrovascular vessels, and reducing myocardial oxygen consumption. Puerarin injection is clinically used to treat cardiovascular and cerebrovascular diseases, retinal vascular diseases, fundus diseases and sudden deafness. With the wide application of kudzu root in clinic, the demand of puerarin is also increasing day by day. [0003] Our country is very rich in kudzu root resources. Therefore, the research and development of an optimized process route for obtaining high-purity puerarin from pueraria is not only conducive to the full and rea...

Claims

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Application Information

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IPC IPC(8): C07D407/04
CPCC07D407/04
Inventor 苗得足黄京山翟乃明王维云
Owner REYOUNG PHARMA
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