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Method for preparing usnic acid

A usnic acid and purpose technology, which is applied in the field of separation and preparation of natural antibiotics, can solve the problems of cumbersome and lengthy process, loss of target product, and lower yield, and achieve the effect of short separation time, strong separation ability and small sample loss

Active Publication Date: 2012-06-20
FEED RESEARCH INSTITUTE CHINESE ACADEMY OF AGRICULTURAL SCIENCES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to multiple recrystallization and silica gel column chromatography will cause a large loss of the target product, the yield is greatly reduced, and the process is cumbersome and lengthy, and the preparation amount is small

Method used

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  • Method for preparing usnic acid
  • Method for preparing usnic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1) Weigh 100 g of Usnea longissima with a mesh size of 20 mesh after crushing, add 600 ml of petroleum ether with a boiling range of 60° C. to 90° C., reflux extraction for 6 hours, and suction filter. Repeat the above reflux extraction step 3 times. The combined filtrates were concentrated to 15 ml at 45° C. under vacuum (vacuum degree of 0 MPa), and allowed to stand at room temperature overnight to obtain a crude extract of usnic acid.

[0020] 2) with the volume ratio being 8: 7: 5: 0.8 the mixed solution that is made up of n-hexane, acetonitrile, ethyl acetate and water is used as two-phase solvent system, adopts high-speed countercurrent chromatograph, the usnic acid that step 1) obtains The crude extract is dissolved in the two-phase solvent system for separation and purification. The specific steps are as follows: after the two-phase solvent system is fully mixed, the phases are separated by standing still, and the two phases are degassed under 100 KHz ultrasoni...

Embodiment 2

[0027] 1) Weigh 100 g of Usnea longissima with a mesh size of 60 mesh after crushing, add 800 ml of petroleum ether with a boiling range of 60-90° C., reflux for extraction for 4 hours, and filter with suction. Repeat the above reflux extraction step 3 times. The combined filtrates were concentrated to 15 ml at 45° C. under vacuum (vacuum degree: 0.01 MPa), and allowed to stand at room temperature overnight to obtain a crude usnic acid extract.

[0028]2) with the volume ratio being 8: 7: 5: 0.8 the mixed solution that is made up of n-hexane, acetonitrile, ethyl acetate and water is used as two-phase solvent system, adopts high-speed countercurrent chromatograph, the usnic acid that step 1) obtains The crude extract is dissolved in the two-phase solvent system for separation and purification. The specific steps are as follows: after the two-phase solvent system is fully mixed, the phases are separated by standing still, and the two phases are degassed under 100 KHz ultrasonic...

Embodiment 3

[0031] Prepare usnic acid according to the same steps as in Example 2, only change the mesh number of Usnea longus in step 1) to 80 mesh, the extraction solvent is ether, consumption 1000mL / time, reflux extraction for 3 hours, extract 2 times , 35 DEG C of vacuum concentrating filtrate to 10ml; In step 2), the amount of usnic acid crude extract is changed to 10 mg, the mobile phase flow rate is changed to 4ml / min, the separation column temperature is 20 DEG C, and the separation column speed is changed to 500rpm.

[0032] According to the same detection conditions as in Example 1, the peak A product was detected by HPLC, and the obtained detection results were the same as in Example 1. The nuclear magnetic detection result of this product is also identical with embodiment 1. From the above NMR and HPLC detection results, it can be seen that the peak A product in the HSCCC spectrogram has a correct structure and is usnic acid with a purity of 99.5% and a yield of 40.08%.

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Abstract

The invention discloses a method for preparing usnic acid. The method comprises the following steps of: 1) crushing usnea longissima and blending the crushed usnea longissima with an organic solvent, and performing refluxing extraction to obtain usnic acid crude extracts; and 2) selecting a two-phase solvent system to separate the usnic acid crude extracts obtained by step 1) by high speed counter-current chromatography to obtain the usnic acid. The method adopts the high speed counter-current chromatography for separating the usnic acid; and compared with conventional experimental preparation method, the method has the obvious advantages of large sample volume at one time, high separation capability, short separation time, small sample loss and synchronous completion of separation and purification. The method provided by the invention is suitable for a high speed counter-current chromatograph with the column capacity of 325ml, and the usnic acid prepared by the method has a purity ofup to 99 percent and a very important application value.

Description

technical field [0001] The invention relates to a method for separating and preparing natural antibiotics in lichen plants, in particular to a method for preparing usnic acid. Background technique [0002] Usnenic acid is one of the main bioactive components of Usnea longus. Usnea longissima (Usnea.longissima) is a lichen plant of the genus Usnea in the family Usnea, also known as tree hanging and canopy grass. It mainly grows in Xinjiang, Inner Mongolia, Yunnan, Gansu, Tibet, Heilongjiang, Jilin, Liaoning and other places. It has the effects of clearing away heat and detoxification, relieving cough and reducing phlegm, and reducing inflammation. Usnic acid shows strong inhibitory effect on Staphylococcus aureus, and also has certain inhibitory effect on E. coli, mold, yeast and pathogenic bacteria. Phlegm, anti-virus, anti-inflammatory, and promote wound healing. [0003] The preparation of usnic acid generally adopts organic solvent extraction, and then undergoes repeat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/91
Inventor 石波梁平迟春艳
Owner FEED RESEARCH INSTITUTE CHINESE ACADEMY OF AGRICULTURAL SCIENCES
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