CN101434530A - Method for extracting alkannin from alkanet - Google Patents
Method for extracting alkannin from alkanet Download PDFInfo
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- CN101434530A CN101434530A CNA2008102096732A CN200810209673A CN101434530A CN 101434530 A CN101434530 A CN 101434530A CN A2008102096732 A CNA2008102096732 A CN A2008102096732A CN 200810209673 A CN200810209673 A CN 200810209673A CN 101434530 A CN101434530 A CN 101434530A
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- shikonin
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Abstract
The invention discloses a method for extracting alkannin from alkanet, which is characterized in that the alkanet is mixed with an aqueous solution containing alcohol in accordance with a certain ratio of material to liquid and put into a pulp refiner for homogenate extraction. Solid-liquid separation is carried out to a mixture obtained after the homogenate to obtain an extracting solution. Solid contents are then mixed with the aqueous solution containing alcohol according to a certain ratio of material to liquid and put into the pulp refiner for the homogenate extraction to obtain an extracting solution. The extracting solutions are merged and then decompression condensed to obtain a crude product of alkannin. The operation technology is mainly characterized by smooth process, simple operation, extraction at room temperature for avoidance of the degradation of alkannin, recyclable reagents used, low energy consumption, low production costs and high yield.
Description
Affiliated technical field:
The present invention relates to the natural product chemistry field, particularly a kind of method of from Radix Arnebiae (Radix Lithospermi), extracting Shikonin.
The principal feature of this operating procedure is the technology smoothness, and is simple to operate, and normal temperature extracts down avoids the Shikonin degraded, the recyclable utilization of agents useful for same, and less energy consumption, production cost is low, the yield height.
Background technology:
Shikonin is as the main medicinal ingredients of Asian puccoon, has multiple pharmacological effect such as hemostasis, antibiotic, anti-inflammatory, antitumor and immunomodulatory, anti-oxidant, liver protecting.Be widely used in tetter such as treatment psoriatic, erythema nodosum, moist macula clinically; Better curative effect is still arranged in burn and scald, acute hepatitis B and gyniatrics simultaneously.Shikonin and derivative thereof all have active group as 5, the structure of quinone etc. on two keys on 8-position phenolic hydroxyl group, the side chain and ester bond, the parent nucleus, prompting extract, preparation and all should prevent that constituent structure from changing when storing or destroyed.According to research reports, Shikonin is higher to the susceptibility of light, oxygen and pH value, extracts temperature and is higher than 60 ℃, acidity-basicity ph〉7, oxygen and supersound extraction time is bigger to composition influence when surpassing 30min.Therefore, how overcoming problem such as Shikonin degraded and isomerization in extracting preparation process, is the important topic that present Shikonin extracts research.So based on above situation, the present invention utilizes the homogenate extraction method to extract Shikonin from the lithospermum euchromum Royle root.
Chinese patent ZL200310124125.7 has introduced Shikonin and iso-alkannin analog derivative make Shikonin and iso-alkannin by the lithium hydroxide hydrolysis method, it is that Shikonin and iso-alkannin ester derivative and 2～200N LiOH are mixed in methanol solution, stirred 24～240 hours, dripping hydrochloric acid is neutralized to system for red, add an amount of and ethyl acetate extraction of entry, extraction liquid is through sodium bicarbonate aqueous solution, water and sodium chloride aqueous solution washing, dried over anhydrous sodium carbonate, decompression and solvent recovery obtains Shikonin and iso-alkannin, it is carried out silica gel column chromatography, obtain pure Shikonin and iso-alkannin.Though this method productive rate height, very high to the purity requirement of raw material, cost is higher.
Publication number is that the Chinese patent of CN1334103 has been introduced supercritical CO
2Abstraction technique extracts the technology of Shikonin from Radix Arnebiae (Radix Lithospermi), it is to utilize CO
2Be special solvent, use is carried agent and is extracted Shikonin under normal temperature and certain pressure.Though this method technology avoids composition to be destroyed without high temperature, owing to adopt supercritical CO
2Extract, be subject to processing quantitative limitation, yield poorly, cost height, fairly largeization of commercial exploitation difficulty production at present.
Publication number is that the Chinese patent of CN1363683 has been introduced Shikonin industrialization extraction process, utilize mould magnetic explosion technology that raw cell is broken, it is that solvent extracts at the diacolation post with the ethanol chloroform that raw material is put into filter bag, filtrate extracts with water after filter bag filters again, utilize pipeline to heat up and reclaim solvent, recovered solvent is added again and continue in the diacolation post to extract, heat drying obtains the Shikonin product.This method equipment requirements height, technology is loaded down with trivial details, and solvent consumption is big, and is consuming time longer.
Publication number is the technology that the Chinese patent of CN1607199 has been introduced basic hydrolysis extraction Shikonin, at first selects for use high-quality Asian puccoon medicinal material to extract with sherwood oil, and extracting solution changes hydrolysis in 0.1～0.5NNaOH solution over to, adds 0.2～0.5N H again
2SO
4Be neutralized to acidity, obtain the red-purple crystallization.Leaching process uses sodium hydroxide in a large number, and the waste water generation is big, difficult treatment; In addition, pH is bigger to its structure influence, and the Shikonin compounds is atropurpureus under alkaline condition, and ultraviolet absorption value obviously reduces, the prepared using rate variance, and yield is low.
Publication number is that the Chinese patent of CN 1720952 has been introduced and exempted to heat extraction process and extract light violet grass, is raw material with light violet grass, and alcohol immersion, liquid grinding, solid-liquid separation, underpressure distillation concentrate, acetic acid ethyl dissolution, cold heavy.This method only can be used fresh Asian puccoon raw material, plucks the processing rapidly of back raw material, perhaps takes strict fresh-keeping measure, and use range is received restriction, need to soak before raw material liquid is pulverized in addition with etoh solvent, and length consuming time, efficient is low.
Summary of the invention:
The object of the present invention is to provide a kind of method of from Radix Arnebiae (Radix Lithospermi), extracting Shikonin, it is characterized in that Radix Arnebiae (Radix Lithospermi) and aqueous solution of alcohol are placed in the refiner by certain solid-liquid ratio, by machinery and fluid power shearing action material is torn and pulverized, material extraction broken and functional component is carried out synchronously, reached quick, strengthen the purpose of extracting the plant functional component.Homogenate extraction method extraction rate is fast, and temperature is low, and energy consumption is low, and purpose composition yield height merges the back concentrating under reduced pressure with extracting solution, obtains the thick product of Shikonin.
Extract the used aqueous solution that contains alcohol in the process of Shikonin and be the volume fraction that contains ethanol, methyl alcohol at 60%～95% the aqueous solution.Used solid-liquid ratio is 1:5～1:30 in the process of extraction Shikonin.2000～10000 rev/mins of refiner revolutions, homogenate extraction time are 1～3 time, and the time that each homogenate is extracted is 3～6 minutes.
Advantage of the present invention is:
1. whole process flow is simple, and is easy to operate, and production cost is low, less energy consumption.
2. adopt homogenate to extract, the extraction efficiency height can effectively be avoided the degradation of Shikonin.
3. all recyclable utilization of agents useful for same, free from environmental pollution, be easy to industrialization.
Specific embodiments:
Below, the present invention will be further detailed with embodiment, but it is not limited to any or the similar example of these embodiment.
Embodiment 1
Get exsiccant Radix Arnebiae (Radix Lithospermi) 50g and place refiner, add 90% ethanolic soln 500ml homogenate by solid-liquid ratio 1:10 and extract 4min, 8000 rev/mins of refiner revolutions, the mixture filtration under diminished pressure, solid adds the 500ml90% ethanolic soln again and extracts 4min, united extraction liquid after the solid-liquid separation, 55 ℃ of concentrating under reduced pressure obtain the thick product 0.82g of Shikonin, and purity is 3.19%.
Embodiment 2
Get exsiccant Radix Arnebiae (Radix Lithospermi) 500g and place refiner, add 80% ethanolic soln 5000ml homogenate by solid-liquid ratio 1:10 and extract 5min, 4000 rev/mins of refiner revolutions, the mixture filtration under diminished pressure that obtains, solid adds the 3000ml80% ethanolic soln again and extracts 5min, united extraction liquid after the solid-liquid separation, 55 ℃ of concentrating under reduced pressure obtain the thick product 8.43g of Shikonin, and purity is 2.95%.
Claims (4)
1. method of from Radix Arnebiae (Radix Lithospermi), extracting Shikonin, it is characterized in that Radix Arnebiae (Radix Lithospermi) and aqueous solution of alcohol mixed by certain solid-liquid ratio and put into refiner homogenate and extract, mixture solid-liquid separation with gained after the homogenate, get extracting solution, solid substance mixed by certain solid-liquid ratio with aqueous solution of alcohol again put into refiner homogenate and extract, extracting solution is merged the back concentrating under reduced pressure, obtain the thick product of Shikonin.
2. according to the described method of from Radix Arnebiae (Radix Lithospermi), extracting Shikonin of claim 1, it is characterized in that: extract the used aqueous solution that contains alcohol in the process of Shikonin and be the volume fraction that contains ethanol, methyl alcohol at 60%～95% the aqueous solution.
3. according to the described method of extracting Shikonin from Radix Arnebiae (Radix Lithospermi) of claim 1, it is characterized in that: used solid-liquid ratio is 1:5～1:30 in the process of extraction Shikonin.
4. according to the described method of extracting Shikonin from Radix Arnebiae (Radix Lithospermi) of claim 1, it is characterized in that: 2000～10000 rev/mins of refiner revolutions, homogenate extraction time are 1～3 time, and the time that each homogenate is extracted is 3～6 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102096732A CN101434530A (en) | 2008-12-12 | 2008-12-12 | Method for extracting alkannin from alkanet |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102096732A CN101434530A (en) | 2008-12-12 | 2008-12-12 | Method for extracting alkannin from alkanet |
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| CN101434530A true CN101434530A (en) | 2009-05-20 |
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| CNA2008102096732A Pending CN101434530A (en) | 2008-12-12 | 2008-12-12 | Method for extracting alkannin from alkanet |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103054925A (en) * | 2012-12-20 | 2013-04-24 | 蚌埠丰原涂山制药有限公司 | Extraction method and obtained extractive and application of alkanet |
| CN103086864A (en) * | 2011-10-31 | 2013-05-08 | 复旦大学 | Shikonin tetramer compound and purpose thereof in pharmacy |
| CN105145596A (en) * | 2015-08-05 | 2015-12-16 | 四川农业大学 | Application of isoflavonoids compound to prepare agricultural bactericide |
| CN106924323A (en) * | 2015-12-30 | 2017-07-07 | 姚萍 | Application of the radix macrotomiae in the medicine for preparing treatment virus B hepatitis |
| CN107929344A (en) * | 2017-12-29 | 2018-04-20 | 吉林省肿瘤医院 | A kind of Asian puccoon compound for being used to preventing and treating laryngocarcinoma |
| CN110302232A (en) * | 2019-08-07 | 2019-10-08 | 中美（河南）荷美尔肿瘤研究院 | A kind of application extracting the method for separating alkanet effective component and its extract and inhibiting in Growth of Colon Cancer Cells drug in preparation |
-
2008
- 2008-12-12 CN CNA2008102096732A patent/CN101434530A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103086864A (en) * | 2011-10-31 | 2013-05-08 | 复旦大学 | Shikonin tetramer compound and purpose thereof in pharmacy |
| CN103086864B (en) * | 2011-10-31 | 2015-01-07 | 复旦大学 | Shikonin tetramer compound and purpose thereof in pharmacy |
| CN103054925A (en) * | 2012-12-20 | 2013-04-24 | 蚌埠丰原涂山制药有限公司 | Extraction method and obtained extractive and application of alkanet |
| CN103054925B (en) * | 2012-12-20 | 2014-07-30 | 安徽丰原药业股份有限公司 | Extraction method and obtained extractive and application of alkanet |
| CN105145596A (en) * | 2015-08-05 | 2015-12-16 | 四川农业大学 | Application of isoflavonoids compound to prepare agricultural bactericide |
| CN106924323A (en) * | 2015-12-30 | 2017-07-07 | 姚萍 | Application of the radix macrotomiae in the medicine for preparing treatment virus B hepatitis |
| CN107929344A (en) * | 2017-12-29 | 2018-04-20 | 吉林省肿瘤医院 | A kind of Asian puccoon compound for being used to preventing and treating laryngocarcinoma |
| CN107929344B (en) * | 2017-12-29 | 2020-07-28 | 吉林省肿瘤医院 | Lithospermum compound composition for preventing and treating laryngeal cancer |
| CN110302232A (en) * | 2019-08-07 | 2019-10-08 | 中美（河南）荷美尔肿瘤研究院 | A kind of application extracting the method for separating alkanet effective component and its extract and inhibiting in Growth of Colon Cancer Cells drug in preparation |
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Open date: 20090520 |