CN102178717A - Method for preparing elephantopus scaber total lactone in elephantopus scaber - Google Patents
Method for preparing elephantopus scaber total lactone in elephantopus scaber Download PDFInfo
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- CN102178717A CN102178717A CN2011101179104A CN201110117910A CN102178717A CN 102178717 A CN102178717 A CN 102178717A CN 2011101179104 A CN2011101179104 A CN 2011101179104A CN 201110117910 A CN201110117910 A CN 201110117910A CN 102178717 A CN102178717 A CN 102178717A
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Abstract
The invention relates to a method for preparing elephantopus scaber total lactone in elephantopus scaber, in particular to a method for preparing elephantopus scaber total lactone from elephantopus scaber by a supercritical extracting method, which comprises the following steps of: crushing whole herbs of the elephantopus scaber, and putting in a supercritical extracting kettle; extracting by using supercritical CO2, and collecting extract in a separating kettle; performing reflux by using petroleum ether to remove lipid soluble impurities, and performing hot melt on derosination matter by using low-carbon alcohol; and adding active carbon for reflux and decolorizing, recovering solvent in destaining solution to proper amount of volume, adding proper amount of water slowly, standing, dissolving crystals out, and filtering to obtain the elephantopus scaber total lactone. The method is environment-friendly, high in efficiency and easy to operate, and a large amount of preparation can be realized.
Description
Technical field:
The invention belongs to the Separation of Natural Products field, especially relate to a kind of method that adopts supercritical extraction prepares the total lactone of Elephantopus scaber L. from Elephantopus scaber L. method.
Background technology:
Elephantopus scaber L. (Elephantopus scaber Linn.) is a Compositae Elephantopus scaber L. platymiscium, Elephantopus scaber L. is only arranged and spends two kinds of Elephantopus scaber L. in vain in China, main product in Zhejiang, ground such as Fujian, Taiwan, Guangdong, Guangxi, Yunnan, Guizhou.Its all herbal medicine of using among the people cures mainly diseases such as flu, tonsillitis, eye conjunctivitis, jaundice, eczema, and this medicine has the effect of heat clearing away, removing heat from blood, detoxifcation, dampness removing.It is reported that Elephantopus scaber L. mainly contains chemical compounds such as sesquiterpene lactones, triterpene, flavone, sterol.Wherein sesquiterpene lactones has the tumor of inhibition and cytotoxicity.
The total lactone of Elephantopus scaber L. is the Elephantopus scaber L. sesquiterpene lactones, mainly comprises lucky agate alkane lactone type, guaianolide type and three kinds of configurations of elemane lactone type.The Elephantopus scaber L. lactone has significant inhibitory effect to vitro human nasopharyngeal carcinoma KB cell and mouse leukemia P388, and deoxidation Elephantopus scaber L. lactone can significantly suppress sarcoma W256, and this belongs to the contained sesquiterpene lactones of other kind of plant also stronger antitumor and cytotoxic activity.The beautiful grade of Liang Qiao studies show that Elephantopus scaber L. sesquiterpene lactones chemical compound scabertopin (1) and isodeoxyelephantopin (2) are in external influence to SMMC-7721, Hela and three kinds of tumor cell proliferations of Caco-2.Find that these two chemical compounds have significant inhibitory effect to three kinds of tumor cell proliferations in 1～100 μ m concentration, and be the doses dependence.
The method of the total lactone of existing extraction Elephantopus scaber L. is less, is by alcohol extraction mostly, the preparation of methods such as ethyl acetate extraction, and consumption of organic solvent is big, and preparation amount is few.Therefore the invention provides a kind of method of supercritical extraction that adopts prepares the total lactone of Elephantopus scaber L. from Elephantopus scaber L., wishes the further research of Elephantopus scaber L. is offered help." the Elephantopus scaber L. The Chemical Constituents " that Huang Ting etc. deliver, document disclosed method is to adopt alcohol extraction, extracting solution adds aqueous dispersion after concentrating, the reuse ethyl acetate extraction, extract gets the various chemical constituents of Elephantopus scaber L. by column chromatography repeatedly, this method manufacturing cycle is long, and preparation amount is few, only is fit to laboratory and prepares on a small quantity.
Summary of the invention:
The technical problem to be solved in the present invention provides a kind of method for preparing the total lactone of Elephantopus scaber L. from Elephantopus scaber L., and this method is simple to operate, and preparation amount is big.
The present invention is achieved by the following technical solutions:
A kind of method for preparing the total lactone of Elephantopus scaber L. from Elephantopus scaber L. is characterized in that comprising following steps:
1) supercritical extraction: the Elephantopus scaber L. herb is pulverized, crossed 20 mesh sieves, place extraction kettle, adopt supercritical CO
2Extraction feeds methanol and participates in extraction as entrainer, collects extract;
2) defat with petroleum ether: add 2～5 times of amount petroleum ether reflux, extract, 1～3 time in above-mentioned extract, the centrifugalize solid-liquid gets the defat thing;
3) purification: with above-mentioned defat thing low-carbon alcohols heating for dissolving, add the active carbon reflux decolour, remove by filter active carbon, destaining solution reclaims solvent to an amount of volume, slowly adds suitable quantity of water, places, and separates out crystal, leach the total lactone of Elephantopus scaber L..
The total lactone of described Elephantopus scaber L. is a sesquiterpene lactones, comprises lucky agate alkane lactone type, guaianolide type and elemane lactone type.
Extraction parameter in the described step 1) is: extraction temperature is 25-40 ℃, and extracting pressure is 15-30MPa, CO
2Flow is 15-25L/h, and the extraction time is 2-4h, and the separation reactor I temperature is 20-30 ℃, and pressure is 6-12MPa, and separation reactor I I temperature is 12-15 ℃, and pressure is 4-6MPa.
Low-carbon alcohols in the described step 3) is C1-C4 alcohol, particular methanol or ethanol.
Good effect of the present invention is:
(1) supercritical extraction, the extraction process power consumption is low, extractant CO
2The source is abundant, cleanliness without any pollution.
(2) solvent system of the present invention's use is comparatively simple, also has low cost, the advantage that the response rate is high.
Further specify the present invention below in conjunction with the specific embodiment, but the scope of protection of present invention is not limited to following embodiment.
The specific embodiment:
Embodiment 1:
Get Elephantopus scaber L. herb 1kg, pulverized 20 mesh sieves, be added in the extraction kettle, adopt supercritical CO
2Extraction feeds 200ml methanol and participates in extraction as entrainer, sets the extraction parameter to be: 40 ℃ of extraction temperature, extracting pressure 15MPa, extraction time 2h, CO
2The amount that feeds is 15L/h, and setting the separation reactor I temperature is 20 ℃, and pressure is 6MPa, separation reactor I I temperature is 12 ℃, and pressure is 4MPa, collects extract in separation reactor I I, add 500ml petroleum ether reflux, extract, 3 times, the centrifugal liquid of removing is again with defat thing methanol heating for dissolving, add the active carbon reflux decolour, destaining solution reclaims solvent to 1/3 of original volume, slowly adds 8 times of water gagings, places, separate out crystal, leach Elephantopus scaber L. total in crystalline esters 10.8g.
Embodiment 2:
Get Elephantopus scaber L. herb 1kg, pulverized 20 mesh sieves, be added in the extraction kettle, adopt supercritical CO
2Extraction feeds 300ml methanol and participates in extraction as entrainer, sets the extraction parameter to be: 25 ℃ of extraction temperature, extracting pressure 30MPa, extraction time 4h, CO
2The amount that feeds is 25L/h, and setting the separation reactor I temperature is 25 ℃, and pressure is 12MPa, separation reactor I I temperature is 15 ℃, and pressure is 6MPa, collects extract in separation reactor I I, add 800ml petroleum ether reflux, extract, 1 time, the centrifugal liquid of removing is again with defat thing ethanol heating for dissolving, add the active carbon reflux decolour, destaining solution reclaims solvent to 1/4 of original volume, slowly adds 10 times of water gagings, places, separate out crystal, leach Elephantopus scaber L. total in crystalline esters 11.2g.
Embodiment 3:
Get Elephantopus scaber L. herb 5kg, pulverized 20 mesh sieves, be added in the extraction kettle, adopt supercritical CO
2Extraction feeds 1.2L methanol and participates in extraction as entrainer, sets the extraction parameter to be: 30 ℃ of extraction temperature, extracting pressure 28MPa, extraction time 2.5h, CO
2The amount that feeds is 18L/h, and setting the separation reactor I temperature is 22 ℃, and pressure is 8MPa, separation reactor I I temperature is 13 ℃, and pressure is 6MPa, collects extract in separation reactor I I, with 2.5L petroleum ether reflux, extract, 2 times, the centrifugal liquid of removing is again with defat thing isopropyl alcohol heating for dissolving, add the active carbon reflux decolour, destaining solution reclaims solvent to 1/4 of original volume, slowly adds 10 times of water gagings, places, separate out crystal, leach the total lactone crystal 4 of Elephantopus scaber L. 8.7g.
Embodiment 4:
Get Elephantopus scaber L. herb 10kg, pulverized 20 mesh sieves, be added in the extraction kettle, adopt supercritical CO
2Extraction feeds 2L methanol and participates in extraction as entrainer, sets the extraction parameter to be: 35 ℃ of extraction temperature, extracting pressure 20MPa, extraction time 3h, CO
2The amount that feeds is 22L/h, and setting the separation reactor I temperature is 25 ℃, and pressure is 10MPa, separation reactor I I temperature is 14 ℃, and pressure is 5MPa, collects extract in separation reactor I I, with 5L petroleum ether reflux, extract, 3 times, the centrifugal liquid of removing is again with defat thing methanol heating for dissolving, add the active carbon reflux decolour, destaining solution reclaims solvent to 1/5 of original volume, slowly adds 7 times of water gagings, places, separate out crystal, leach Elephantopus scaber L. total in crystalline esters 100.3g.
Claims (4)
1. method for preparing the total lactone of Elephantopus scaber L. from Elephantopus scaber L. is characterized in that comprising following steps:
1) supercritical extraction: the Elephantopus scaber L. herb is pulverized, crossed 20 mesh sieves, place extraction kettle, adopt supercritical CO
2Extraction feeds methanol and participates in extraction as entrainer, collects extract;
2) defat with petroleum ether: add 2～5 times of amount petroleum ether reflux, extract, 1～3 time in above-mentioned extract, the centrifugalize solid-liquid gets the defat thing;
3) purification: with above-mentioned defat thing low-carbon alcohols heating for dissolving, add the active carbon reflux decolour, remove by filter active carbon, destaining solution reclaims solvent to an amount of volume, slowly adds suitable quantity of water, places, and separates out crystal, leach the total lactone of Elephantopus scaber L..
2. a kind of method for preparing the total lactone of Elephantopus scaber L. from Elephantopus scaber L. as claimed in claim is characterized in that the total lactone of described Elephantopus scaber L. is a sesquiterpene lactones, comprises lucky agate alkane lactone type, guaianolide type and elemane lactone type.
3. a kind of method that from Elephantopus scaber L., prepares the total lactone of Elephantopus scaber L. as claimed in claim, it is characterized in that the extraction parameter in the described step 1) is: extraction temperature is 25-40 ℃, extracting pressure is 15-30MPa, CO
2Flow is 15-25L/h, and the extraction time is 2-4h, and the separation reactor I temperature is 20-30 ℃, and pressure is 6-12MPa, and separation reactor I I temperature is 12-15 ℃, and pressure is 4-6MPa.
4. a kind of method for preparing the total lactone of Elephantopus scaber L. from Elephantopus scaber L. as claimed in claim is characterized in that the low-carbon alcohols in the described step 3) is C1-C4 alcohol, particular methanol or ethanol.
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| CN2011101179104A CN102178717A (en) | 2011-05-06 | 2011-05-06 | Method for preparing elephantopus scaber total lactone in elephantopus scaber |
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| CN2011101179104A CN102178717A (en) | 2011-05-06 | 2011-05-06 | Method for preparing elephantopus scaber total lactone in elephantopus scaber |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114129558A (en) * | 2021-11-12 | 2022-03-04 | 暨南大学附属第一医院（广州华侨医院） | Application of sesquiterpene lactone compounds in preparation of chemotherapeutic drug antitumor synergist or drug resistance reversal agent |
-
2011
- 2011-05-06 CN CN2011101179104A patent/CN102178717A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114129558A (en) * | 2021-11-12 | 2022-03-04 | 暨南大学附属第一医院（广州华侨医院） | Application of sesquiterpene lactone compounds in preparation of chemotherapeutic drug antitumor synergist or drug resistance reversal agent |
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Application publication date: 20110914 |