CN102827180A - Extraction method of gutolactone - Google Patents
Extraction method of gutolactone Download PDFInfo
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- CN102827180A CN102827180A CN 201210368435 CN201210368435A CN102827180A CN 102827180 A CN102827180 A CN 102827180A CN 201210368435 CN201210368435 CN 201210368435 CN 201210368435 A CN201210368435 A CN 201210368435A CN 102827180 A CN102827180 A CN 102827180A
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- guyana
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- incense wood
- lactone
- liquid
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- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
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Abstract
The invention discloses an extraction method of gutolactone, belonging to the field of natural drug chemistry. The method comprises the following steps: mixing the raw material Simaba guianensis Aubl. bark with an ethanol solution, carrying out negative-pressure cavitation suspension solid-liquid extraction to obtain an extract, concentrating, carrying out counter-current extraction on the concentrated solution, separating the concentrated extract by high-speed counter-current chromatography, concentrating the fraction under reduced pressure by using n-hexane-chloroform-methanol-water as a solvent system, and recrystallizing with acetone to obtain the high-purity gutolactone. By adopting the negative-pressure cavitation suspension solid-liquid extraction and high-speed counter-current chromatography separation techniques, the invention is efficient and environment-friendly, and is suitable for industrial large-scale production.
Description
Technical field
The invention belongs to the extractive technique field of crude substance, relate to the process for extracting of a kind of Guyana incense wood lactone.
Background technology
Guyana incense wood lactone, CAS 152369-48-7 is incense wood from Simarubaceae (Simaroubaceae) Guyana
Simaba guianensisAubl. separate a kind of quassia active component that obtains, molecular formula C in the bark
25H
32O
9, molecular weight 476.52.Discover that Guyana incense wood lactone has antimalarial active, external IC50 (ng/ml): Indochina W-2 strain (4.0), SierraLeone D-6 strain (4.1) to plasmodium falciparum.
Through the document retrieval, domestic the discovery as yet adopts negative pressure-cavitation homogenous solid-liquid phase liquid-solid extraction and high speed adverse current chromatogram stripping technique to prepare the relevant report of the commercial run of Guyana incense wood lactone.
Summary of the invention
The process for extracting that the purpose of this invention is to provide a kind of Guyana incense wood lactone of efficient, environmental protection.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
The tree bark powder of (1) getting Guyana incense wood is broken into meal, and after doubly measuring (V/W) ethanolic soln with 8-12 and mixing, cavitation suspendible 20-50min carries out the negative pressure-cavitation homogenous solid-liquid phase liquid-solid extraction 1-2 time, obtains extracting solution;
(2) extracting solution concentrates the back and uses volume ratio to carry out counter-current extraction as acetone-ethyl acetate mixture of 1:2, the collection extraction liquid, and decompression and solvent recovery gets liquid concentrator;
(3) liquid concentrator is used the high speed adverse current chromatogram separation and purification, with normal hexane-chloroform-methanol-water two-phase solvent system, on be stationary phase mutually, be moving phase mutually down, collect composition according to collection of illustrative plates, the elutriant rotary evaporation is concentrated, promptly get Guyana incense wood lactone coarse-grain;
(4) recrystallization: Guyana incense wood lactone coarse-grain is used acetone recrystallization, and lyophilize obtains crystalline esters in the incense wood of faint yellow Guyana.
Ethanolic soln concentration is 80% described in the said step (1).
Normal hexane-chloroform-methanol-water volume ratio is (10-13) in the said step (3): (9-13): (13-16): (6-9).
The invention has the beneficial effects as follows: 1) weak point simple to operate, consuming time is easy to industrialization and amplifies;
2) adopt the method for negative pressure-cavitation homogenous solid-liquid phase liquid-solid extraction that the ricinine in the plant material is extracted, the time is short, and efficient is high; 3) adopt high speed adverse current chromatogram to separate Guyana incense wood lactone, the loss of sepn process product-free, efficient, preparation cycle is short.
Embodiment:
To combine embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment 1:
Get the bark 1000g of Guyana incense wood, be ground into meal, after the ethanolic soln of 10L80% mixes; Cavitation suspendible 50min carries out the negative pressure-cavitation homogenous solid-liquid phase liquid-solid extraction 2 times, obtains extraction liquid; Extraction liquid reclaim under reduced pressure reagent gets medicinal extract, adds the extraction cat head, uses volume ratio to carry out counter-current extraction as acetone-ETHYLE ACETATE of 1:2; By adding from the extraction tower bottom with feed liquid throughput ratio 2:1; Make two to mix the completion extraction mutually, collect the extraction liquid that the top collection has Guyana incense wood lactone, the reclaim under reduced pressure extraction agent gets liquid concentrator.Get normal hexane, chloroform, methyl alcohol, water by the 13:10:14:5 mixed, standing demix is got and is pumped into chromatotube mutually; Open high-speed counter-current chromatograph, the adjustment rotating speed is 850rpm, simultaneously pumping into the 3ml/min flow velocity down; Inject liquid concentrator, the UV-detector monitoring, the monitoring wavelength is 222nm; Collect flow point, behind the concentrating under reduced pressure, promptly get Guyana incense wood lactone coarse-grain; Guyana incense wood lactone coarse-grain is used acetone recrystallization, and lyophilize obtains crystalline esters in the incense wood of faint yellow Guyana, content 96.46%.
Embodiment 2:
Get the bark 1000g of Guyana incense wood, be ground into meal, after the ethanolic soln of 12L80% mixes; Cavitation suspendible 40min carries out the negative pressure-cavitation homogenous solid-liquid phase liquid-solid extraction 1 time, obtains extraction liquid; Extraction liquid reclaim under reduced pressure reagent gets medicinal extract, adds the extraction cat head, uses volume ratio to carry out counter-current extraction as acetone-ETHYLE ACETATE of 1:2; By adding from the extraction tower bottom with feed liquid throughput ratio 2:1; Make two to mix the completion extraction mutually, collect the extraction liquid that the top collection has Guyana incense wood lactone, the reclaim under reduced pressure extraction agent gets liquid concentrator.Get normal hexane, chloroform, methyl alcohol, water by the 11:13:16:9 mixed, standing demix is got and is pumped into chromatotube mutually; Open high-speed counter-current chromatograph, the adjustment rotating speed is 800rpm, simultaneously pumping into the 3ml/min flow velocity down; Inject liquid concentrator, the UV-detector monitoring, the monitoring wavelength is 222nm; Collect flow point, behind the concentrating under reduced pressure, promptly get Guyana incense wood lactone coarse-grain; Guyana incense wood lactone coarse-grain is used acetone recrystallization, and lyophilize obtains crystalline esters in the incense wood of faint yellow Guyana, content 94.93%.
Embodiment 3:
Get the bark 1000g of Guyana incense wood, be ground into meal, after the ethanolic soln of 8L80% mixes; Cavitation suspendible 20min carries out the negative pressure-cavitation homogenous solid-liquid phase liquid-solid extraction 2 times, obtains extraction liquid; Extraction liquid reclaim under reduced pressure reagent gets medicinal extract, adds the extraction cat head, uses volume ratio to carry out counter-current extraction as acetone-ETHYLE ACETATE of 1:2; By adding from the extraction tower bottom with feed liquid throughput ratio 2:1; Make two to mix the completion extraction mutually, collect the extraction liquid that the top collection has Guyana incense wood lactone, the reclaim under reduced pressure extraction agent gets liquid concentrator.Get normal hexane, chloroform, methyl alcohol, water by the 13:9:15:7 mixed, standing demix is got and is pumped into chromatotube mutually; Open high-speed counter-current chromatograph, the adjustment rotating speed is 950rpm, simultaneously pumping into the 2.5ml/min flow velocity down; Inject liquid concentrator, the UV-detector monitoring, the monitoring wavelength is 222nm; Collect flow point, behind the concentrating under reduced pressure, promptly get Guyana incense wood lactone coarse-grain; Guyana incense wood lactone coarse-grain is used acetone recrystallization, and lyophilize obtains crystalline esters in the incense wood of faint yellow Guyana, content 95.98%.
Embodiment 4:
Get the bark 1000g of Guyana incense wood, be ground into meal, after the ethanolic soln of 8L80% mixes; Cavitation suspendible 50min carries out the negative pressure-cavitation homogenous solid-liquid phase liquid-solid extraction 2 times, obtains extraction liquid; Extraction liquid reclaim under reduced pressure reagent gets medicinal extract, adds the extraction cat head, uses volume ratio to carry out counter-current extraction as acetone-ETHYLE ACETATE of 1:2; By adding from the extraction tower bottom with feed liquid throughput ratio 2:1; Make two to mix the completion extraction mutually, collect the extraction liquid that the top collection has Guyana incense wood lactone, the reclaim under reduced pressure extraction agent gets liquid concentrator.Get normal hexane, chloroform, methyl alcohol, water by the 10:9:13:6 mixed, standing demix is got and is pumped into chromatotube mutually; Open high-speed counter-current chromatograph, the adjustment rotating speed is 850rpm, simultaneously pumping into the 3ml/min flow velocity down; Inject liquid concentrator, the UV-detector monitoring, the monitoring wavelength is 222nm; Collect flow point, behind the concentrating under reduced pressure, promptly get Guyana incense wood lactone coarse-grain; Guyana incense wood lactone coarse-grain is used acetone recrystallization, and lyophilize obtains crystalline esters in the incense wood of faint yellow Guyana, content 96.45%.
Claims (3)
1. the process for extracting of Guyana incense wood lactone is characterized in that may further comprise the steps:
The tree bark powder of (1) getting Guyana incense wood is broken into meal, and after doubly measuring (V/W) ethanolic soln with 8-12 and mixing, cavitation suspendible 20-50min carries out the negative pressure-cavitation homogenous solid-liquid phase liquid-solid extraction 1-2 time, obtains extracting solution;
(2) extracting solution concentrates the back and uses volume ratio to carry out counter-current extraction as acetone-ethyl acetate mixture of 1:2, the collection extraction liquid, and decompression and solvent recovery gets liquid concentrator;
(3) liquid concentrator is used the high speed adverse current chromatogram separation and purification, with normal hexane-chloroform-methanol-water two-phase solvent system, on be stationary phase mutually, be moving phase mutually down, collect composition according to collection of illustrative plates, the elutriant rotary evaporation is concentrated, promptly get Guyana incense wood lactone coarse-grain;
(4) recrystallization: Guyana incense wood lactone coarse-grain is used acetone recrystallization, and lyophilize obtains crystalline esters in the incense wood of faint yellow Guyana.
2. the process for extracting of a kind of Guyana as claimed in claim 1 incense wood lactone is characterized in that ethanolic soln concentration is 80% described in the said step (1).
3. the process for extracting of a kind of Guyana as claimed in claim 1 incense wood lactone is characterized in that normal hexane-chloroform-methanol in the said step (3)-water volume ratio is (10-13): (9-13): (13-16): (6-9).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210368435 CN102827180A (en) | 2012-09-28 | 2012-09-28 | Extraction method of gutolactone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210368435 CN102827180A (en) | 2012-09-28 | 2012-09-28 | Extraction method of gutolactone |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102827180A true CN102827180A (en) | 2012-12-19 |
Family
ID=47330515
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201210368435 Pending CN102827180A (en) | 2012-09-28 | 2012-09-28 | Extraction method of gutolactone |
Country Status (1)
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|---|---|
| CN (1) | CN102827180A (en) |
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2012
- 2012-09-28 CN CN 201210368435 patent/CN102827180A/en active Pending
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Application publication date: 20121219 |