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Technique for producing usnic acid

A production process, the technology of usnic acid, is applied in organic chemistry, antibacterial drugs, and medical raw materials derived from lichens, etc. It can solve the problems of many types of organic solvents, low utilization rate of raw materials, and serious cross-mixing, etc. The effect of large-scale industrial production, improving utilization rate and improving extraction rate

Inactive Publication Date: 2007-10-10
NANJING AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Technical Problem In order to overcome the disadvantages of complex process, excessive solvent consumption, many types of organic solvents, serious cross-mixing, low raw material utilization rate, high cost and low work efficiency in the existing traditional technology, the present invention provides a Convenient and effective production process of usnic acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1. Put 500kg of Usnea longiflora washed and dried into an extraction percolation tank, add 5 times the volume of ethyl acetate, heat and circulate reflux for extraction for 8 hours, control the temperature at 75°C, and concentrate the filtrate to 200L. The density of the ethyl acetate usnic acid extract obtained by concentration is 0.25g / cm 3 ;

[0018] Separate the 200L ethyl usnic acid extract in 4 50L white plastic buckets, and place them in a cold room at -10℃ for overnight crystallization. Filter the next day to obtain the orange-yellow usnic acid crude crystals. The crude acid was recrystallized with ethyl acetate, the temperature was maintained at 50℃~60℃, the ratio of material to liquid was 1:4, 92% pure usnic acid was detected;

[0019] The 92% pure usnic acid was dissolved in chloroform to remove the chloroform insoluble matter, the material-liquid ratio was 1:2, frozen overnight at a low temperature of -10°C for crystallization, crystallized and detected ...

Embodiment 2

[0020] Example 2. Put 200kg of usnea longifolia that was washed and air-dried into an extraction percolation tank, add 5 times the amount of ethyl acetate, heat and circulate reflux for extraction for 7.5 hours, control the temperature at 80°C, and concentrate the filtrate to 100L; The 100L ethyl acetate usnic acid extract was divided into two 50L white plastic buckets, and placed in a cold room at -10℃ for overnight crystallization. The orange-yellow usnic acid crystals were obtained by filtration the next day. The crude usnic acid Using the same method as Example 1, it was heated to dissolve and recrystallized with ethyl acetate, and it was detected that 94% pure usnic acid was obtained; the 94% pure usnic acid was dissolved in chloroform to remove the chloroform insoluble matter, crystallized and detected to obtain 97% fine pine Dildo.

Embodiment 3

[0021] Example 3. Put 100kg of Usnea longi being washed and air-dried into an extraction percolation tank, add 5 times the amount of ethyl acetate, heat and circulate reflux for extraction for 9 hours, control the temperature at 60°C, and concentrate the filtrate to 50L; The 50L ethyl acetate usnic acid extract was placed in a 50L white plastic bucket, and placed in a cold room at -10℃ for overnight crystallization. The orange-yellow usnic acid crystals were obtained by filtration the next day. The crude usnic acid The same method was used to dissolve and recrystallize with ethyl acetate to obtain 95% pure usnic acid; the 95% pure usnic acid was dissolved in chloroform to remove the chloroform insoluble matter, and 99% refined usnic acid was crystallized and detected.

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PUM

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Abstract

This invention relates to a process for extracting usnic acid from Usnea longissima. The process comprises: adding dried Usnea longissima in a percolator, adding 3-5 volume times of ethyl acetate, heating to 60-80 deg.C, extracting, concentrating, freezing for crystallization, filtering, recrystallizing to obtain 90-95% usnic acid, dissolving in chloroform to remove insoluble impurities, and crystallizing to obtain higher than 98% usnic acid. The method has such advantages as high extraction rate (higher than 85%), high usnic acid utility, saved biological resources, simple process, low energy consumption and is suitable for mass production.

Description

Technical field [0001] The invention relates to a production process of usnic acid, which belongs to the field of traditional Chinese medicine, and is dedicated to the process for extracting the organic acid usnic acid from the Chinese medicinal crude drug plant Usnea longum. technical background [0002] Usnic acid is an organic acid widely found in Usnea lichens. It has antibacterial properties, inhibits plant growth, antiviral properties, affects bacterial toxins and bacteriophage activity, and has other anti-malaria and vaginal trichomonas effects. . Studies have shown that the antibacterial spectrum of usnic acid is mainly Gram-positive bacteria and Mycobacterium tuberculosis. Usnic acid in the test tube has a strong antibacterial effect on pneumococcus, hemolytic streptococcus, diphtheria bacillus, and tubercle bacillus. The inhibitory concentration is 1 to 5 μg / ml, and 50 μg / ml can completely inhibit the growth of bacteria. . The inhibition of Staphylococcus aureus is slig...

Claims

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Application Information

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IPC IPC(8): C07D307/91A61K36/09A61P31/04A61P31/06
Inventor 何新华刘兆普刘玲赵耕毛章睿琳章贻琴
Owner NANJING AGRICULTURAL UNIVERSITY
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