Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for purifying and refining glycyrrhetic acid from liquorice by microwave auxiliary cloud point extraction

A microwave-assisted, glycyrrhizic acid technology is applied in the direction of medical preparations containing active ingredients, pharmaceutical formulas, steroids, etc., to achieve the effects of simple experimental operation, easy refining, and low cost

Inactive Publication Date: 2010-12-08
INST OF PROCESS ENG CHINESE ACAD OF SCI
View PDF1 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Combining microwave extraction and cloud point extraction to separate glycyrrhizic acid has never been reported

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Put 20 grams of licorice powder into the reaction vessel of the microwave-assisted extraction equipment, add 200 ml of water, control the temperature at 80°C, and microwave extraction for 5 minutes. The content of glycyrrhizic acid in the filtrate accounted for 3.3% of the mass of licorice. Add 10ml of GX-080 to fully mix and dissolve, adjust the pH of the mixed solution to 2.2 with a concentration of 10wt% hydrochloric acid, and then heat to 75°C in microwave for phase extraction. After 30 minutes, glycyrrhizic acid is enriched in the micelle phase formed by the surfactant In; Separate the micelle phase and add 30ml of water to dissolve it, adjust the pH of the mixed solution to 7.0 with a 5wt% aqueous sodium hydroxide solution, then heat again to a cloud point temperature of 75°C for phase separation, take the aqueous phase solution to precipitate and dry with hydrochloric acid The crude glycyrrhizic acid was obtained at a content of 47%. The crude glycyrrhizic acid w...

Embodiment 2

[0027] Put 20 grams of licorice powder into the reaction vessel of the microwave-assisted extraction equipment, add 200 ml of water, control the temperature at 90° C., and microwave extraction for 5 minutes. The content of glycyrrhizic acid in the filtrate accounted for 3.6% of the mass of licorice. Add 10ml Triton X-100 to fully dissolve it, adjust the pH of the mixed solution to 2.5 with a concentration of 10wt% hydrochloric acid, and then heat it to 75℃ in microwave for phase extraction. After 30 minutes, the glycyrrhizic acid is enriched in the micelle phase formed by the surfactant In; Separate the micelle phase and add 30ml of water to dissolve it, adjust the pH of the mixed solution to 7.8 with a 5wt% aqueous sodium hydroxide solution, then heat it to a cloud point temperature of 75°C for phase separation, take the aqueous phase solution to precipitate and dry with hydrochloric acid The crude glycyrrhizic acid was obtained at a content of 54%. Crude glycyrrhizic acid wa...

Embodiment 3

[0029] Put 20 grams of licorice powder into the reaction vessel of the microwave-assisted extraction equipment, add 200 ml of water, control the temperature at 90° C., and microwave extraction for 5 minutes. The content of glycyrrhizic acid in the filtrate accounted for 3.6% of the mass of licorice. Add 10ml Triton X-100 to fully dissolve it, adjust the pH of the mixed solution to 2.5 with a concentration of 10wt% sulfuric acid, and then heat the water bath to 70°C for phase extraction. After 60 minutes, the glycyrrhizic acid is enriched in the micelles formed by the surfactant Separate the micelle phase and add 30ml of water to dissolve it, adjust the pH of the mixed solution to 7.8 with an aqueous solution of sodium hydroxide with a concentration of 5wt%, and then heat it to a cloud point temperature of 70°C for phase separation. Take the aqueous phase solution and precipitate it with sulfuric acid. After drying, the crude glycyrrhizic acid is obtained with a content of 51%. ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to the medicine chemical engineering field, in particular to a method for purifying and refining glycyrrhetic acids from liquorices by microwave assistant cloud point extraction. The method is as follows: firstly, by the microwave assistant extraction method, glycyrrhetic acids are extracted from liquorices quickly and efficiently; secondly, cloud point extraction is made bya glue ball solution formed by nonionic surfactants, and the pH value is adjusted to between 1.5 and 3.0, and after the glue ball solution is heated to the cloud point temperature, the glue ball solution is divided into two phases of a water phase and a glue ball phase, and the glycyrrhetic acids are mainly in the glue ball phase; by taking water as a solution, the pH value of the mixed solution is adjusted to between 6.0 and 8.0, and the cloud point back washing is made again, finally the water phase solution containing abundant glycyrrhetic acids is obtained, and coarse glycyrrhetic acids are obtained after the acidification and precipitation of the water phase solution, and the ethanol with high concentration is added to coarse glycyrrhetic acids, after heat dissolution and filtering, the glycyrrhetic acid tripotassium salt is obtained; the glycyrrhetic acid tripotassium salt is added with and dissolved in glacial acetic acids, and is crystallized and separated out, and thus the white glycyrrhetic acid monopotassium salt with high purity is obtained, the purity of the glycyrrhetic acid monopotassium salt is more than 90 percent. The method has the advantages of simple operation, no volatile organic solvent in the process of extraction and high enrichment and purification efficiency.

Description

Technical field [0001] The invention relates to the field of pharmaceutical chemicals, in particular to a method for purifying and refining glycyrrhizic acid from licorice by microwave-assisted cloud point extraction. Background technique [0002] Pure potassium glycyrrhizinate is an important fine chemical product in the world. It is widely used in medicine, food and cosmetics as a raw material or additive. [0003] At present, the traditional method of extracting glycyrrhizic acid is heat reflux or decoction with water. This method has the disadvantages of long extraction time, low extraction rate, and more impurities in the product. The production processes of refined glycyrrhizic acid mainly include: acid precipitation crystallization method, ion exchange method and macroporous resin adsorption method. The direct acid precipitation crystallization method generally requires multiple recrystallizations, with complex steps and low yield; using ion exchange resins and adsorption ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00A61K36/484
Inventor 刘会洲孙晨田庆来安震涛
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com