Method for extracting volatile oil from usnea and simultaneously extracting usnea polysaccharide and usnic acid

A technology of usnea polysaccharide and volatile oil, which is applied in the field of extracting volatile oil from usnea and simultaneously extracting usnea polysaccharide and usnenic acid, can solve the problems of not perfect extraction method of usnea polysaccharide, achieve low cost and strong operability , The effect of simple process

Active Publication Date: 2019-04-05
HUNAN HUACHENG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no perfect method for ex

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] The method of extracting volatile oil from usnea:

[0067] (1) Reflux extraction: pulverize 10kg of dried usnea longum to a particle size of 2mm, add 150L of 6# extraction solvent oil, reflux extraction at 80°C for 4h, and filter to obtain the extract;

[0068] (2) Silica gel column chromatography separation: the extract obtained in step (1) is installed on a chromatography column with silica gel at a flow rate of 1.0 BV / h (the amount of silica gel is 2L, and the column height to diameter ratio is 6:1) , Collect the effluent and concentrate at 75°C under normal pressure to obtain 412.60g of volatile oil.

[0069] Detected by distillation method, the mass content of the volatile oil in the product obtained in the example of the present invention is 92.1%, and the yield is 95%.

[0070] Simultaneous extraction of usnea polysaccharide:

[0071] After filtering the 13kg residue (wet weight) obtained in step (1), after recovering the 6# solvent oil at 85°C, add 150kg of hot water at ...

Embodiment 2

[0077] The method of extracting volatile oil from usnea:

[0078] (1) Reflux extraction: pulverize 20kg of dried Usnea longifolia to a particle size of 1mm, add 200L n-hexane, reflux extraction at 70°C for 5h, and filter to obtain the extract;

[0079] (2) Alumina column chromatography separation: The extract obtained in step (1) is installed on a chromatography column with alumina at a flow rate of 0.5 BV / h (the amount of alumina is 3L, and the height-to-diameter ratio of the column is 8 1) Collect the effluent and concentrate at 85°C under normal pressure to obtain 797.43g of volatile oil.

[0080] Detected by distillation method, the mass content of the volatile oil in the product obtained in the example of the present invention is 93.3%, and the yield is 93%.

[0081] The method of extracting usnea polysaccharide at the same time:

[0082] After filtering the 26kg residue (wet weight) obtained from step (1), after recovering the n-hexane at 87°C, add 200kg of hot water at 90°C, sti...

Embodiment 3

[0088] The method of extracting volatile oil from usnea:

[0089] (1) Reflux extraction: pulverize 15kg of dried Usnea longifolia to a particle size of 2mm, add 180L of 6# extraction solvent oil, reflux extraction at 75°C for 4.5h, and filter to obtain the extract;

[0090] (2) Reversed-phase silica gel column chromatography separation: The extract obtained in step (1) is installed on a chromatographic column equipped with reversed-phase silica gel at a flow rate of 0.6 BV / h (the amount of reversed-phase silica gel is 1.5L, and the height of the column is 1.5L. The diameter ratio is 5:1), the effluent is collected and concentrated at 80°C under normal pressure to obtain 578.83g of volatile oil.

[0091] Detected by distillation method, the mass content of the volatile oil in the product obtained in the example of the present invention is 95.2%, and the yield is 92%.

[0092] Simultaneous extraction of usnea polysaccharide:

[0093] After filtering the 19.5kg extract residue (wet weight...

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Abstract

The invention discloses a method for extracting volatile oil from usnea and simultaneously extracting usnea polysaccharide and usnic acid. The method for extracting volatile oil from usnea includes the following steps: (1) reflux extraction: crushing dried usnea, adding an organic solvent, reflux extracting, and filtering to obtain an extracting solution; (2) column chromatography separation: arranging a chromatography column filled with a filler on the extracting solution obtained in the step (1), collecting an effluent liquid, and concentrating to obtain the volatile oil. The invention further discloses a method for simultaneously extracting usnea polysaccharide and usnea acid. In the volatile oil, usnea polysaccharide and usnea acid products obtained by the method, the mass content of the volatile oil, usnea polysaccharide and usnea acid can reach 95.2%, 97.5% and 99.7% respectively, and the yield can reach 95%, 95% and 97% respectively. The method can comprehensively utilize usnearesources, has high product yield, high purity, simple process, strong operability, low cost and little pollution, so that the method is suitable for industrial production.

Description

Technical field [0001] The invention specifically relates to a method for extracting volatile oil from usnea and simultaneously extracting usnea polysaccharide and usnic acid. Background technique [0002] Usnea (scientific name: Usnea diffracta Vain ) Also known as: female dill, pine parasitic, loose, canopy grass, snow wind cane, mountain dried noodles, long beard grass, Lysimachia, Guan Gong's beard, canopy grass, tree hanging, flying centipede, pine hair, sea breeze vine, stone Silk thread, flying mountain wings, fairy hair, golden stilt, cloud grass, old king's beard, beard grass, tea beard, mountain dragon, stone beard, belong to the Usnea family plant, divided into two kinds: Usnea and Usnea , Born in the deep mountains of old branches or high mountain rocks, into hanging filaments. [0003] In traditional Chinese medicine, Usnea is mostly used for coughing and phlegm, tuberculosis, malaria, headache, red eyes, carbuncle, scrofula, scrofula, mastoid carbuncle, traumatic bl...

Claims

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Application Information

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IPC IPC(8): C11B1/04C11B1/10C08B37/00C07D307/91
CPCC11B1/04C11B1/10C07D307/91C08B37/0003
Inventor 龙伟岸黄华学
Owner HUNAN HUACHENG BIOTECH
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