Method for extracting high-purity scutellarin from breviscpini

A technology for scutellarin and scutellarin, which is applied in the field of extraction and separation of plant active ingredients, can solve the problems of unclear ingredients, low scutellarin content, no relevant literature reports, etc., and achieves the effect of preventing the influence of heat

Active Publication Date: 2011-07-27
YUNNAN PHYTOPHARML +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Breviscapine is an active ingredient of flavonoids extracted from breviscapine herb, mainly scutellarin, also known as scutellarin, chemically named 4', 5, 6-trihydroxyflavone-7-O-glucose Aldehydroside, the scutellarin raw material drug currently purchased from the market is analyzed by HPLC, and the content of scutellarin is between 80-90%. Its various preparations are clinically used to treat cardiovascular and cerebrovascular diseases, with definite curative effect However, the stability of its injection is poor, and its ingredients other than breviscapine are not clear, which increases the uncontrollable safety of breviscapine injection, so it is of great significance to extract and separate high-purity breviscapine from breviscapine
[0003] In order to solve the technical problem of low content of scutellarin in scutellarin for a long time, patent applications 200410062573.3; 200410040182.1; 200410040352.6; 200410079583.8; The content of scutellarin prepared by the technology is high, reaching more than 98%. Patent applications 200710066155.5 and 200710065713.6 use macroporous adsorption resin to purify scutellarin, but the above patents are all refined with commercially available scutellarin and require a large amount of However, there is no relevant literature report on the extraction and separation process of high-purity scutellarin with stable quality directly extracted from scutellaria breviscapine

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 100kg of dried wild scutellaria breviscapus grass, add 800L of 75% methanol, soak and extract 3 times, extract for 12 hours each time, combine the extracts, filter, recover the methanol solution under reduced pressure to a relative density of 1.12, add water to dilute, the amount of water added is the amount of scutellaria scutellaria 3 times of the diluent, heat the diluent to 80°C, add 20L of ZTC1+1 clarifying agent B component with a concentration (mass volume ratio) of 1%, stir while adding until precipitation precipitates, continue stirring for 5min, and keep it standing at 80°C 1h, add 15L of ZTC1+1 clarifier A component with a concentration (mass volume ratio) of 1%, stir while adding until flocculent precipitates precipitate, continue stirring for 2min, let stand for 1h, filter, and cool the filtrate to below 30°C , put on 250KgAB-8 macroporous adsorption resin column, elute with water, discard the eluate of the first column volume, collect the eluate of 2-5...

Embodiment 2

[0026] Take 100kg of dried scutellaria breviscapus grass, add 600L of 80% ethanol, and extract twice with ethanol under reflux for 2 hours each time, combine the extracts, filter, recover the alcohol solution under reduced pressure to a relative density of 1.07, add water to dilute, and add water for breviscapine Add 30L of 101 fruit juice clarifier with a concentration (mass volume ratio) of 5% to the diluent, stir until precipitation precipitates, continue to stir for 5min, let stand for 1h, filter, and 250KgD101 macropores on the filtrate Adsorption resin column, elute with water, discard the eluate in the first to second column volume, collect the eluate in 3-7 column volumes, concentrate with nanofiltration membrane, the temperature of the eluent is 26°C, and the operating pressure is, 1Mpa, concentrate until there is no water out of the outlet of the nanofiltration membrane, add acetone 4 times the volume of the concentrate to the concentrate, let it stand overnight, filt...

Embodiment 3

[0028] Take 100kg of the above-ground part of fresh home-grown breviscapine, add 600L of 70% ethanol, soak and extract three times at 50°C, extract for 5 hours each time, combine the extracts, filter, recover the alcohol under reduced pressure to a relative density of 1.15, add water to dilute, and add water It is 5 times of the feeding amount of scutellaria breviscapus, the diluent is heated to 80°C, and 40L of the ZTC1+1 clarifying agent B component with a concentration (mass volume ratio) of 1% is added, and stirred while adding until there is precipitation, and the stirring is continued for 3 minutes. Insulate and stand at 80°C for 1 hour, add 25L of ZTC1+1 clarifying agent A component with a concentration (mass volume ratio) of 1%, stir while adding until flocculent precipitates are precipitated, continue stirring for 2 minutes, let stand for 1 hour, filter, and the filtrate Cool to below 30°C, put on a 250KgHPD-100 macroporous adsorption resin column, elute with water, di...

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PUM

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Abstract

The invention relates to a method for extracting high-purity scutellarin from breviscapin. The method comprises the following steps: the breviscapin raw material is extracted by using organic solvent, the filtrate is added with clarifying agent for coagulation and clarifying, the coagulated and clarified filtrate is absorbed by macroporous absorbent resin and is eluted with water, the water eluent is concentrated through a reverse osmosis membrane or nanofiltration membrane, the concentrated solution is added with the organic solvent for standing and precipitation, the sediment is filtered and collected, the aqueous solution of the organic solvent is added and stirred to be suspendible, and after standing a night, the sediment is filtered, collected and washed to be near-neutral with water to obtain the high-purity scutellarin after drying. The alkali is not used in the entire process, the clarifier is used for removing the water insoluble matter, the impurity removal is carried out by using the macroporous absorbent resin, the concentration is carried out by using the reverse osmosis membrane or the nanofiltration membrane, the scutellarin plant salt is prevented from being heated and degraded in water, the content of the prepared scutellarin can reach above 97 percent, the quality is stable, the process is simple and the pollution is little.

Description

technical field [0001] The invention belongs to the technical field of extraction and separation of effective plant components, in particular to a method for extracting and separating high-purity scutellarin from scutellaria scutellaria. Background technique [0002] Erigeron breviscapus (vant) Hard, -Mass is the dry whole herb of Compositae plant Erigeron breviscapus (vant) Hard, -Mass, also known as Erigeron breviscapus, East chrysanthemum. Distributed in Yunnan, Sichuan, Guizhou, Guangxi, Hunan and other places. Cold in nature, slightly bitter, has the effects of dispelling cold and relieving the exterior, expelling wind and dampness, promoting blood circulation and removing blood stasis, dredging meridian and activating collaterals, reducing inflammation and relieving pain. Once included in the "Chinese Pharmacopoeia" 1977 edition. Breviscapine is an active ingredient of flavonoids extracted from breviscapine herb, mainly scutellarin, also known as scutellarin, chemica...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/07C07H1/08
Inventor 周敏武正才赵锋宁何玉清李文黄春球
Owner YUNNAN PHYTOPHARML
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