Method for preparing psoralen and isopsoralen or extract containing psoralen and isopsoralen

A technology for isopsoralen and psoralen, which is applied in the field of extraction and separation of traditional Chinese medicine, can solve the problems of long time required for medicinal materials and limited amount of pure product, and achieves the effects of short preparation period, low cost and simple process

Active Publication Date: 2013-01-16
CHINA RESOURCES SANJIU MEDICAL & PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the traditional process, this method can obtain crude isopsoralen while obtaining psoralen crystals. The process is simple and the cycle is short, but it takes a long time to crush the medicinal material and the amount of pure product obtained is limited.

Method used

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  • Method for preparing psoralen and isopsoralen or extract containing psoralen and isopsoralen
  • Method for preparing psoralen and isopsoralen or extract containing psoralen and isopsoralen
  • Method for preparing psoralen and isopsoralen or extract containing psoralen and isopsoralen

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] Embodiment 1, preparation comprises the extract of psoralen and isopsoralen and each monomer

[0075] Preparation steps:

[0076] Step i): take 1 kg of psoraleae medicinal material, extract twice with water under reflux, the first water consumption is 8 times of the medicinal material amount, the second water consumption is 6 times of the medicinal material amount, each time for 1.5 hours, and the combined extract Concentrate to 1:1 with the weight of medicinal materials, which is 1L, to obtain a concentrated solution;

[0077] Step ii): adding acid (hydrochloric acid) to the obtained concentrated solution so that the concentration of the acid (in terms of hydrogen ions) reaches 1.5 mol / L, and heating and hydrolyzing at 95-100° C. for 30 minutes;

[0078] Step iii): The hydrolyzate is eluted with water on the macroporous adsorption resin column (D101) to remove impurities, and then eluted with a 95% aqueous ethanol solution, and the ethanol eluate is collected, conce...

Embodiment 2

[0081] Example 2, preparation of extracts and monomers comprising psoralen and isopsoralen

[0082] Carried out with reference to the method of Example 1. in

[0083] Step i) refluxing and extracting the water once for 5 hours, the water consumption is 10 times the amount of medicinal materials, and the combined extract is concentrated to 1:1 with the weight of medicinal materials;

[0084] The acid used in the step ii) is sulfuric acid, so that the concentration of the acid (in terms of hydrogen ions) reaches 3mol / L, and it is heated and hydrolyzed at 90 to 100°C for 15 minutes;

[0085] In step iii), the hydrolyzate is eluted with water on the macroporous adsorption resin column (AB-8) to remove impurities, then eluted with absolute ethanol, and the ethanol eluate is collected, concentrated, and dried to obtain a compound containing psoralen and 110 g of the extract of this example of isopsoralen;

[0086] iv) Dissolve / suspend 10 g of the extract obtained in step iii) w...

Embodiment 3

[0088] Example 3, preparation of extracts and monomers comprising psoralen and isopsoralen

[0089] Carried out with reference to the method of Example 1. in

[0090] Step i) refluxing and extracting the middle water for 4 times, each time for 0.5 hours, each time the water consumption is 8 times the amount of the medicinal material, and the combined extract is concentrated to 1:1 with the weight of the medicinal material;

[0091] The acid used in the step ii) is nitric acid, the concentration of the acid (in terms of hydrogen ions) reaches 0.5mol / L, and the hydrolysis is carried out at 90-100° C. for 60 minutes;

[0092] In step iii), the hydrolyzate is eluted with water on a macroporous adsorption resin column (NKA) to remove impurities, then eluted with an aqueous ethanol solution with a concentration of 90%, and the ethanol eluate is collected, concentrated, and dried to obtain psoralen-containing and 83.3 g of the present embodiment extract of isopsoralen;

[0093] ...

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Abstract

The invention relates to a method for preparing psoralen and isopsoralen or an extract containing psoralen and isopsoralen. Particularly the method comprises the steps of (i) conducting backflow extraction on fructus psoraleae medicinal materials by using water, and concentrating a combined extracting solution to obtain a concentrated solution; (ii) adding acid in the obtained concentrated solution, heating and hydrolyzing; (iii) eluting hydrolysate on a macroporous adsorption resin by using water to remove impurities, eluting by using ethanol water solution with concentration larger than 50%, collecting an ethanol eluant, and concentrating or optionally drying further to obtain the extract containing psoralen and isopsoralen; and (iv) optionally subjecting the extract obtained in the step (iii) to a silicagel column, eluting by using an organic solvent, collecting psoralen fraction and isopsoralen fraction, and removing the solvent to respectively obtain psoralen and isopsoralen. The method is simple in operation, short in production period, high in yield, less in pollution and applicable to industrialization mass production.

Description

technical field [0001] The invention relates to the technical field of extraction and separation of traditional Chinese medicines, in particular to a method for separating and preparing active ingredients psoralen and isopsoralen in psoralen or an extract containing them. Background technique [0002] Psoralen is the dried and mature fruit of Psoralea corylifolia L., a leguminous plant. It was first seen in "Kaibao Materia Medica". It is distributed in Shanxi, Shaanxi, Anhui and other places. Antidiarrheal effect. Modern chemical research shows that psoralen mainly contains glycosides, coumarins, flavonoids, and monoterpene phenolic components, which have antibacterial, antioxidative, antiviral, antitumor, and immune-enhancing activities. At present, the development and utilization of psoralen has attracted the attention of pharmaceutical workers, and psoralen nasal drops, psoralen dripping pills, compound psoralen tincture for treating vitiligo, etc. have been reported. C...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/04
Inventor 高秀梅王跃飞彭四威刘二伟熊文朱彦杨静
Owner CHINA RESOURCES SANJIU MEDICAL & PHARMA
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