CN102649711A - Extracting method for drumstick phenanthrene - Google Patents
Extracting method for drumstick phenanthrene Download PDFInfo
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- CN102649711A CN102649711A CN2011100452823A CN201110045282A CN102649711A CN 102649711 A CN102649711 A CN 102649711A CN 2011100452823 A CN2011100452823 A CN 2011100452823A CN 201110045282 A CN201110045282 A CN 201110045282A CN 102649711 A CN102649711 A CN 102649711A
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Abstract
The invention relates to an extracting method for drumstick phenanthrene, which comprises the following steps of: crushing dendrobium plant drugs; performing ultrasonic or backflow extraction by taking 70-95% alcohol solution; concentrating the extracting solution, thereby obtaining a crude extract; dissolving the crude extract with 8-20 times of 20% alcohol; taking macroreticular resin from supernate; decolorizing by adding active carbon into eluent injection; filtering the active carbon; concentrating, thereby obtaining precipitate; washing the precipitate with petroleum ether, thereby obtaining crude product; separating and purifying the crude product by adopting a HSCCC (High Speed Counter Current Chromatography) method; and reducing pressure and drying the effluent, thereby obtaining the product. The method is simple in process for producing the drumstick phenanthrene; the purity is high; and the preparation volume is large.
Description
Technical field:
The present invention relates to the luxuriant and rich with fragrance process for extracting of a kind of drumstick, especially relate to a kind of macroporous resin and luxuriant and rich with fragrance method of high speed adverse current chromatogram separation and purification drumstick of adopting.
Background technology:
In recent years, the research of bibenzyl and the effect of luxuriant and rich with fragrance compounds anti-tumor activity is just receiving foreign scholar's great attention, and these compounds are to the muroid L of vitro culture
1210The gathering of tubulin and mitotic division, cell strain, multiple human body tumor cell line such as A-549, MCF-7, HT-29, SKMEL-5, MLM, SK-OV-3, HL-60 all have restraining effect.The auspicious grade of Malaysian selects for use liver cancer, ehrlich carcinoma to compose as knurl; To the ethanol extraction of Dendrobium chrysotoxum and hair orchid is plain, hair orchid is luxuriant and rich with fragrance, drumstick is luxuriant and rich with fragrance carries out anti-tumor activity research; The result shows: Dendrobium chrysotoxum ethanol extraction and three monomers all have anti-tumor activity in various degree; The strongest with the plain effect of hair orchid to rat liver cancer, its tumour inhibiting rate is 50.82%; The strongest with the luxuriant and rich with fragrance effect of drumstick to ehrlich carcinoma, its tumour inhibiting rate is 62.25%.Results of study such as Wang Tianshan show that dihydro bibenzyl in the Dendrobium chrysotoxum and luxuriant and rich with fragrance compounds have restraining effect in various degree to the growth of tumor cell line.Dendrobium is big a genus, and China product Dendrobium plant is more than 60 kinds, and from the Dendrobium plant that germ plasm resource is so enriched, the antitumor drug with clinical value and commercial value is sought in screening, is undoubtedly work very promising and very attractive.
The drumstick phenanthrene is a kind of from one of isolated active ingredient of Chinese herbs of Dendrobium plant, in State Intellectual Property Office's coordinate indexing and CNKI retrieval, does not find the technical study of the Sino-Philippines compounds of extraction separation Dendrobium.
Drumstick luxuriant and rich with fragrance (chrysotoxene), chemical name: 2-hydroxyl-1,5,6, the 7-tetramethoxy is luxuriant and rich with fragrance; Molecular formula: C
18H
18O
5, molecular weight 314.34; Be colourless plate crystal, mp.177-178 ℃ (sherwood oil-chloroform).
Summary of the invention:
The object of the present invention is to provide the luxuriant and rich with fragrance process for extracting of a kind of drumstick.
The object of the invention is realized through following technical proposals:
The process for extracting that a kind of drumstick is luxuriant and rich with fragrance, it is characterized in that may further comprise the steps: with the Dendrobium plant is raw material, pulverizes, and adds the ultrasonic or refluxing extraction of 70-95% ethanol; Repeat 2-3 time, united extraction liquid, extracting solution obtains crude extract after concentrating, after crude extract is dissolved with 8-20 20% ethanol commentaries on classics doubly; Get macroporous adsorbent resin on the supernatant, with water, 30% ethanol, 80% ethanol elution, collect 80% ethanol eluate successively, add injection medical active carbon decoloring; The filtering gac is concentrated into the 1/15-1/10 of original volume, throw out, get bullion with the petroleum ether throw out; Separate with high speed adverse current chromatogram, collect elute, evaporated under reduced pressure promptly gets product.
Said Dendrobium plant is selected one or more mixing among the stem of noble dendrobium Dendrobium primulinum Lindl. of heralding spring, Dendrobium chrysotoxum Dendrobiumchrysotoxum Lidl., the Dendrobium williamsonii Day et Reichb. F. Dendrobium williamsonii Day et Reichb.F. for use.
The 10-20 that said extraction solvent consumption is a material quantity doubly.
Said macroporous resin is selected D101 or AB-8 type macroporous adsorbent resin for use, and the post blade diameter length ratio is 1: 5-1: 7, and the absorption flow rate control is at 2-5L/h.
Said injection medicinal carbon consumption is the 2-5 ‰ of solution amount.
It is heptane-ETHYLE ACETATE-acetone that said high speed adverse current chromatogram separates solvent systems, and ratio is (5-10): (1-3): (4-7).
Beneficial effect of the present invention: (1) from the Dendrobium plant, extracts first and enrichment obtains high purity drumstick phenanthrene; (2) high, the suitable suitability for industrialized production of this preparation technology's yield can be used for preparing various medicines or healthcare products with antitumor action.
Embodiment:
Below in conjunction with embodiment the present invention is described in further detail, but embodiment of the present invention is not limited thereto.
Embodiment 1:
Get the Dendrobium vegetable drug and pulverize, get 10kg and drop in the 200L pilot scale extractor, added 100L80% ethanolic soln refluxing extraction 2 hours; The extracting supernatant extracts 2 times united extraction liquid again with similarity condition; Extracting solution is concentrated into small volume, obtains crude extract, after crude extract is dissolved with 10 times of 20% ethanolic soln commentaries on classics; Get supernatant and add D101 macroporous resin column (post blade diameter length ratio 1: 7) absorption, absorption flow velocity is 2.5L/h, water, 30% ethanol, 80% ethanol elution successively after the absorption end; Collect 80% ethanol eluate, add 45g injection medical active carbon decoloring, the filtering gac; Be concentrated into 1/13 of original volume, get throw out, get 6.0g powdery bullion with the petroleum ether throw out; Get heptane, ETHYLE ACETATE, acetone and placed separating funnel to mix in 5: 1: 4 by volume, standing demix separates phase up and down; Getting mutually and to be stationary phase, be moving phase down mutually, and it is for use in mutually under being dissolved in right amount to get above-mentioned powdery bullion; Open the countercurrent chromatography appearance, go into moving phase with the 2ml/min flow pump, and through the sampling valve continuous sample introduction; The control rotating speed is 750r/min; Regularly collect the luxuriant and rich with fragrance flow point of drumstick through detector, the concentrating under reduced pressure evaporate to dryness gets the luxuriant and rich with fragrance 912mg of drumstick, performance liquid detection level 98.2%.
Embodiment 2:
Get the Dendrobium vegetable drug and pulverize, get 10kg and drop in the 200L pilot scale extractor, added 120L90% ethanolic soln refluxing extraction 1.5 hours; The extracting supernatant extracts 3 times united extraction liquid again with similarity condition; Extracting solution is concentrated into small volume, obtains crude extract, after crude extract is dissolved with 15 times of 20% ethanolic soln commentaries on classics; Get supernatant and add AB-8 macroporous resin column (post blade diameter length ratio 1: 5) absorption, absorption flow velocity is 3.5L/h, water, 30% ethanol, 80% ethanol elution successively after the absorption end; Collect 80% ethanol eluate, add 40.5g injection medical active carbon decoloring, the filtering gac; Be concentrated into 1/12 of original volume, get throw out, get 6.2g powdery bullion with the petroleum ether throw out; Get heptane, ETHYLE ACETATE, acetone and placed separating funnel to mix in 10: 3: 7 by volume, standing demix separates phase up and down; Getting mutually and to be stationary phase, be moving phase down mutually, and it is for use in mutually under being dissolved in right amount to get above-mentioned powdery bullion; Open the countercurrent chromatography appearance, go into moving phase with the 3ml/min flow pump, and through the sampling valve continuous sample introduction; The control rotating speed is 700r/min; Regularly collect the luxuriant and rich with fragrance flow point of drumstick through detector, the concentrating under reduced pressure evaporate to dryness gets the luxuriant and rich with fragrance 906mg of drumstick, performance liquid detection level 98.4%.
Embodiment 3:
Get the Dendrobium vegetable drug and pulverize, get 10kg and drop in the 200L pilot scale extractor, added 140L70% ethanolic soln refluxing extraction 1.5 hours; The extracting supernatant extracts 2 times united extraction liquid again with similarity condition; Extracting solution is concentrated into small volume, obtains crude extract, after crude extract is dissolved with 8 times of 20% ethanolic soln commentaries on classics; Get supernatant and add AB-8 macroporous resin column (post blade diameter length ratio 1: 6) absorption, absorption flow velocity is 2.0L/h, water, 30% ethanol, 80% ethanol elution successively after the absorption end; Collect 80% ethanol eluate, add 75g injection medical active carbon decoloring, the filtering gac; Be concentrated into 1/10 of original volume, get throw out, get 6.4g powdery bullion with the petroleum ether throw out; Get heptane, ETHYLE ACETATE, acetone and placed separating funnel to mix in 6: 2: 5 by volume, standing demix separates phase up and down; Getting mutually and to be stationary phase, be moving phase down mutually, and it is for use in mutually under being dissolved in right amount to get above-mentioned powdery bullion; Open the countercurrent chromatography appearance, go into moving phase with the 1ml/min flow pump, and through the sampling valve continuous sample introduction; The control rotating speed is 800r/min; Regularly collect the luxuriant and rich with fragrance flow point of drumstick through detector, the concentrating under reduced pressure evaporate to dryness gets the luxuriant and rich with fragrance 904mg of drumstick, performance liquid detection level 99.2%.
Embodiment 4:
Get the Dendrobium vegetable drug and pulverize, get 10kg and drop in the 200L pilot scale extractor, added 200L85% ethanolic soln refluxing extraction 3 hours; The extracting supernatant extracts 2 times united extraction liquid again with similarity condition; Extracting solution is concentrated into small volume, obtains crude extract, after crude extract is dissolved with 17 times of 20% ethanolic soln commentaries on classics; Get supernatant and add D101 macroporous resin column (post blade diameter length ratio 1: 7) absorption, absorption flow velocity is 5.0L/h, water, 30% ethanol, 80% ethanol elution successively after the absorption end; Collect 80% ethanol eluate, add 60g injection medical active carbon decoloring, the filtering gac; Be concentrated into 1/15 of original volume, get throw out, get 5.8g powdery bullion with the petroleum ether throw out; Get heptane, ETHYLE ACETATE, acetone and placed separating funnel to mix in 5: 3: 6 by volume, standing demix separates phase up and down; Getting mutually and to be stationary phase, be moving phase down mutually, and it is for use in mutually under being dissolved in right amount to get above-mentioned powdery bullion; Open the countercurrent chromatography appearance, go into moving phase with the 3ml/min flow pump, and through the sampling valve continuous sample introduction; The control rotating speed is 750r/min; Regularly collect the luxuriant and rich with fragrance flow point of drumstick through detector, the concentrating under reduced pressure evaporate to dryness gets the luxuriant and rich with fragrance 918mg of drumstick, performance liquid detection level 98.3%.
Embodiment 5:
Get the Dendrobium vegetable drug and pulverize, get 10kg and drop in the 200L pilot scale extractor, added 160L95% ethanolic soln refluxing extraction 1 hour; The extracting supernatant extracts 3 times united extraction liquid again with similarity condition; Extracting solution is concentrated into small volume, obtains crude extract, after crude extract is dissolved with 20 times of 20% ethanolic soln commentaries on classics; Get supernatant and add D101 macroporous resin column (post blade diameter length ratio 1: 5) absorption, absorption flow velocity is 3.0L/h, water, 30% ethanol, 80% ethanol elution successively after the absorption end; Collect 80% ethanol eluate, add 52.5g injection medical active carbon decoloring, the filtering gac; Be concentrated into 1/11 of original volume, get throw out, get 6.1g powdery bullion with the petroleum ether throw out; Get heptane, ETHYLE ACETATE, acetone and placed separating funnel to mix in 8: 2: 5 by volume, standing demix separates phase up and down; Getting mutually and to be stationary phase, be moving phase down mutually, and it is for use in mutually under being dissolved in right amount to get above-mentioned powdery bullion; Open the countercurrent chromatography appearance, go into moving phase with the 2ml/min flow pump, and through the sampling valve continuous sample introduction; The control rotating speed is 800r/min; Regularly collect the luxuriant and rich with fragrance flow point of drumstick through detector, the concentrating under reduced pressure evaporate to dryness gets the luxuriant and rich with fragrance 908mg of drumstick, performance liquid detection level 98.7%.
Claims (6)
1. the luxuriant and rich with fragrance process for extracting of a drumstick, it is characterized in that may further comprise the steps: with the Dendrobium plant is raw material, pulverizes, and adds the ultrasonic or refluxing extraction of 70-95% ethanol; Repeat 2-3 time, united extraction liquid, extracting solution obtains crude extract after concentrating, after crude extract is dissolved with 8-20 20% ethanol commentaries on classics doubly; Get macroporous adsorbent resin on the supernatant, with water, 30% ethanol, 80% ethanol elution, collect 80% ethanol eluate successively, add injection medical active carbon decoloring; The filtering gac is concentrated into the 1/15-1/10 of original volume, throw out, get bullion with the petroleum ether throw out; Separate with high speed adverse current chromatogram, collect elute, evaporated under reduced pressure promptly gets product.
2. the process for extracting that drumstick as claimed in claim 1 is luxuriant and rich with fragrance is characterized in that said Dendrobium plant selects one or more mixing among the stem of noble dendrobium Dendrobium primulinum Lindl. of heralding spring, Dendrobium chrysotoxum Dendrobium chrysotoxum Lindl., the Dendrobium williamsonii Day et Reichb. F. Dendrobiumwilliamsonii Day et Reichb.F. for use.
3. the process for extracting that drumstick as claimed in claim 1 is luxuriant and rich with fragrance is characterized in that 10-20 that said extraction solvent consumption is a material quantity doubly.
4. the process for extracting that drumstick as claimed in claim 1 is luxuriant and rich with fragrance is characterized in that said macroporous resin selects D101 or AB-8 type macroporous adsorbent resin for use, and the post blade diameter length ratio is 1: 5-1: 7, and the absorption flow rate control is at 2-5L/h.
5. the process for extracting that drumstick as claimed in claim 1 is luxuriant and rich with fragrance is characterized in that said injection medicinal carbon consumption is the 2-5 ‰ of solution amount.
6. the process for extracting that drumstick as claimed in claim 1 is luxuriant and rich with fragrance is characterized in that it is heptane-ETHYLE ACETATE-acetone that said high speed adverse current chromatogram separates solvent systems, and ratio is (5-10): (1-3): (4-7).
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| CN2011100452823A CN102649711A (en) | 2011-02-25 | 2011-02-25 | Extracting method for drumstick phenanthrene |
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| CN2011100452823A CN102649711A (en) | 2011-02-25 | 2011-02-25 | Extracting method for drumstick phenanthrene |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109400732A (en) * | 2018-10-13 | 2019-03-01 | 安发（福建）生物科技有限公司 | A method of preparing dendrobium polysaccharide and dendrobium nobile phenanthrol simultaneously from dendrobium candidum |
| CN110118844A (en) * | 2019-04-24 | 2019-08-13 | 云南省农业科学院质量标准与检测技术研究所 | A kind of preparation method and applications of high-purity hair orchid phenanthrene |
| CN111333491A (en) * | 2020-02-28 | 2020-06-26 | 沈阳药科大学 | Preparation method of phenanthrene compound in dendrobium officinale |
-
2011
- 2011-02-25 CN CN2011100452823A patent/CN102649711A/en active Pending
Non-Patent Citations (4)
| Title |
|---|
| 林萍等: "石斛属植物药理活性研究进展", 《中草药》 * |
| 许有威等: "高速逆流色谱结合大孔树脂从龙胆中快速分离高纯度龙胆苦苷", 《中国中药杂志》 * |
| 马国祥等: "反相高效液相色谱法测定18种石斛类中药中chrysotoxene,erianin及chrysotoxine的含量", 《中国药科大学学报》 * |
| 马国祥等: "鼓槌石斛化学成分的研究", 《药学学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109400732A (en) * | 2018-10-13 | 2019-03-01 | 安发（福建）生物科技有限公司 | A method of preparing dendrobium polysaccharide and dendrobium nobile phenanthrol simultaneously from dendrobium candidum |
| CN110118844A (en) * | 2019-04-24 | 2019-08-13 | 云南省农业科学院质量标准与检测技术研究所 | A kind of preparation method and applications of high-purity hair orchid phenanthrene |
| CN111333491A (en) * | 2020-02-28 | 2020-06-26 | 沈阳药科大学 | Preparation method of phenanthrene compound in dendrobium officinale |
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Application publication date: 20120829 |