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Method for extracting usnic acid from sun-lo

A technology of usnic acid and usnea, applied in the direction of organic chemistry, can solve the problems of great harm to operators, excessive use of organic toxic reagents, serious environmental pollution, etc., to solve the problem of difficult resin adsorption, reduce costs, and ensure safe operation of personnel sex high effect

Inactive Publication Date: 2011-02-16
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Natural extraction is mainly extracted from Usnea, the main method is to use ethyl acetate, acetone alcohol solution or ethanol benzene solution as extraction solvent, ultrasonic, percolation or reflux extraction, silica gel column separation or recrystallization with different organic solvents. The method uses too many organic toxic reagents, which will cause great harm to operators, serious environmental pollution, and high cost

Method used

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  • Method for extracting usnic acid from sun-lo

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take Usnea raw material, pick and remove impurities and crush it, weigh 1kg and put it into a stainless steel multifunctional small extraction tank, take 130g of sodium bicarbonate and add appropriate amount of water to dissolve, take ethanol to make a 6L90% solution, add it to the extraction tank and reflux for 1 hour, extract three times, and combine The extract reclaims ethanol, adds an appropriate amount of water to disperse to obtain the upper column liquid, takes 200ml001×7 cationic resin, treats it with 2% sodium hydroxide solution and 3% hydrochloric acid solution successively, washes the neutral column with water, and treats 500mlD101 macroporous resin in the same way, Two resin columns are connected in series, the upper column solution is added to the resin column, the flow rate is controlled at 3L / h, and the adsorption is repeated 3 times. After the adsorption is completed, 4.5L of 50% ethanol solution is taken to elute the macroporous resin column, and the elu...

Embodiment 2

[0026] Take Usnea raw material, pick and remove impurities and crush, weigh 1kg and put it into a stainless steel multi-functional small extraction tank, take 200g sodium carbonate and add appropriate amount of water to dissolve, take ethanol to make a 10L 70% solution, add it to the extraction tank and reflux for 1 hour, extract three times, and combine the extraction Recover ethanol from liquid, add appropriate amount of water to disperse to get upper column liquid, take 200ml D301 cationic resin, treat with 2% sodium hydroxide solution and 3% hydrochloric acid solution successively, wash neutral column with water, treat 500ml AB-8 macroporous resin in the same way , two resin columns are connected in series, the upper column solution is added to the resin column, the flow rate is controlled at 4L / h, and the adsorption is repeated 4 times. After the adsorption is completed, 2.5L of 90% ethanol solution is taken to elute the macroporous resin column, and the eluent recovers eth...

Embodiment 3

[0028] Take Usnea raw material, pick and remove impurities and crush it, weigh 1kg and put it into a stainless steel multifunctional small extraction tank, take 150g of sodium bicarbonate and add appropriate amount of water to dissolve, take ethanol and configure it into a 15L85% solution, add it to the extraction tank for reflux for 2 hours, and extract twice, Combine the extracts to recover ethanol, add an appropriate amount of water to disperse to obtain the upper column liquid, take 200ml D113 cationic resin, treat it with 2% sodium hydroxide solution and 3% hydrochloric acid solution successively, wash the neutral column with water, and treat 500ml X-5 large Porous resin, two resin columns connected in series, add the upper column liquid into the resin column, control the flow rate at 5L / h, repeat the adsorption 5 times, after the adsorption is completed, take 3.5L of 750% ethanol solution to elute the macroporous resin column, and the eluent is recovered Ethanol to 40% le...

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Abstract

The invention relates to a method for extracting usnic acid from sun-lo, which comprises the following steps: pulverizing sun-lo, adding alkaline alcohol solution, carrying out reflux extraction for 2-3 times, recycling ethanol from the extracting solution, adsorbing by adding to cationic resin macroporous resin series columns, eluting with 50-90% ethanol, concentrating the eluent until the alcohol crystal concentration reaches 30-50%, and refluxing anhydrous ethanol to recrystallize. The method for producing usnic acid can reduce the pollution and lower the production cost. The invention is suitable for industrial production.

Description

[0001] Technical field: [0002] The invention relates to a method for purifying usnic acid from usnea, in particular to a method for purifying usnic acid with a macroporous resin. Background technique: [0003] Usnic acid is also called lichenic acid [0004] Molecular formula: C 18 h 16 o 7 ; [0005] Molecular weight: 344.32 [0006] Molecular formula: [0007] [0008] Physical and chemical properties: melting point 192-204°C, soluble in chloroform, slightly soluble in ethanol, ethyl acetate, acetone, hardly soluble in petroleum ether. Its sodium salt is soluble in water and ethanol. [0009] Usnic acid is a broad-spectrum antibiotic that has a strong inhibitory effect on most Gram-positive bacteria and can also inhibit the growth of Mycobacterium tuberculosis. Usnic acid also has inhibitory effect on protozoa and vaginal trichomonas. Clinically, it has certain curative effect against malaria. It has a certain effect on trauma, burns and skin diseases, cervix ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/91
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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