CN103265414A - Preparation method of confusarin - Google Patents
Preparation method of confusarin Download PDFInfo
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- CN103265414A CN103265414A CN2013101944646A CN201310194464A CN103265414A CN 103265414 A CN103265414 A CN 103265414A CN 2013101944646 A CN2013101944646 A CN 2013101944646A CN 201310194464 A CN201310194464 A CN 201310194464A CN 103265414 A CN103265414 A CN 103265414A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention discloses a preparation method of confusarin. The preparation method is simple and convenient to operate and less in pollution. The preparation method comprises the following steps of: 1) crushing dendrobium fimbriatum as a raw material to form 20 to 80 meshes, extracting the dendrobium fimbriatum in a supercritical CO2 extraction tank at the extraction temperature of 30 to 60 DEG C and under the pressure of 20 to 30Mpa for 1 to 4 hours, wherein the flow of the CO2 is from 1 to 5ml/min for the material per gram; dissolving an extractant by using trichloromethane, filtering and recycling a reagent, thereby obtaining a crude extract; and 2) serving a stationary phase of the crude extract as a fixing phase and a bottom phase of the crude extract as a mobile phase by taking the trichloromethane, methanol and water as a solvent system and performing purification via high-speed counter-current chromatography, wherein the rotational speed of a host machine is from 700 to 1000 rpm and the flow rate of the mobile phase is from 1 to 4ml/min; collecting a distillate according to the illustration; and drying the distillate under reduced pressure, thereby obtaining the confusarin. The prepared confusarin is high in product purity, so that industrialized amplification is easy to realize.
Description
Technical field
The invention belongs to the Natural Medicine Chemistry field, particularly relate to a kind of preparation method of hair orchid phenanthrene.
Background technology
Hair orchid phenanthrene (confusarin) chemical name 2,7-dihydroxyl 1,5,6-trimethoxy phenanthrene, colourless plate crystal, fusing point 191.1-192 ℃, molecular weight 300, molecular structural formula:
The hair orchid phenanthrene is phenolic compound, is soluble in organic solvents such as chloroform, acetone, methyl alcohol, and is atomic water-soluble.The auspicious grade of Malaysian discovers that hair orchid phenanthrene (eonfusarin) has different restraining effect to the growth of the tumor cell line K562 of vitro culture, its cell proliferation inhibition rate is that 50% drug level is respectively 0.0065,5.34,0.32,46.15 μ g/ml hair orchid phenanthrene (eonfusarin) and also has anti-oxidant activity, and is strong than BHA to the antioxygenic activity of ferric iron thiocyanate-.The existing method for preparing drum hair orchid phenanthrene adopts normal pressure, conventional reagent to extract more, and extraction efficiency is low, and the subsequent purification complex steps, and is seriously polluted.The method that adopts as the auspicious people of grade of Malaysian is alcohol reflux and then adopts silica gel column chromatography that eluting solvent is many, and is seriously polluted, is difficult to amplify produce.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of easy and simple to handle, preparation method of polluting little hair orchid phenanthrene.
The objective of the invention is to realize by the following technical solutions: a kind of preparation method of hair orchid phenanthrene is characterized in that comprising following steps:
1) with stem of Eyeshaped Dendrobium raw material pulverizing 20-80 order, places CO
2Extract CO in the supercritical extraction jar
2Flow is the 1-5ml/min/g raw material, extraction temperature 30-60 ℃, and pressure 20-30Mpa, extraction time 1-4h, extract dissolves with chloroform, filters, and reclaims reagent and gets crude extract;
2) above-mentioned crude extract is solvent systems with chloroform, methyl alcohol, water, gets the phase that fixes mutually, is mutually moving phase to adopt the high speed adverse current chromatogram purifying down, engine speed 700-1000rpm, flow rate of mobile phase 1-4ml/min collects flow point according to collection of illustrative plates, and the flow point drying under reduced pressure namely.
Step 2) chloroform in, methyl alcohol, water for the solvent ratio are: 5-10:2-4:4-9.
Adopt present method to prepare the hair orchid phenanthrene, the extraction efficiency height, purification step is simple to operation, and pollutes for a short time, is easy to industrialization and amplifies.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1:
With stem of Eyeshaped Dendrobium raw material pulverizing 40 orders, get 2kg, place the supercritical extraction jar to extract, feed CO
2Flow is the 3ml/min/g raw material, 40 ℃ of extraction temperature, and pressure 25Mpa, extraction time 2h, extract dissolves with chloroform, filters, and reclaims chloroform and gets crude extract.Get chloroform, methyl alcohol, water and mix by 5:2:5, get the upper strata and inject the high speed adverse current chromatogram pipe phase that fixes, take off layer and do moving phase, flow velocity 2ml/min, engine speed 800rpm, moving phase dissolving crude extract, sample introduction, collect flow point according to collection of illustrative plates, preparation continuously, flow point merges concentrate drying, De Maolanfei 1.5g, detect content 98.2% through HPLC.
Embodiment 2:
With stem of Eyeshaped Dendrobium raw material pulverizing 80 orders, get 2kg, place the supercritical extraction jar to extract, feed CO
2Flow is the 1ml/min/g raw material, 30 ℃ of extraction temperature, and pressure 20Mpa, extraction time 3h, extract dissolves with chloroform, filters, and reclaims chloroform and gets crude extract.Get chloroform, methyl alcohol, water and mix by 7:3:9, get the upper strata and inject the high speed adverse current chromatogram pipe phase that fixes, take off layer and do moving phase, flow velocity 3ml/min, engine speed 900rpm, moving phase dissolving crude extract, sample introduction, collect flow point according to collection of illustrative plates, preparation continuously, flow point merges concentrate drying, De Maolanfei 1.2g, detect content 95.7% through HPLC.
Embodiment 3:
With stem of Eyeshaped Dendrobium raw material pulverizing 60 orders, get 2kg, place the supercritical extraction jar to extract, feed CO
2Flow is the 6ml/min/g raw material, 35 ℃ of extraction temperature, and pressure 27Mpa, extraction time 2h, extract dissolves with chloroform, filters, and reclaims chloroform and gets crude extract.Get chloroform, methyl alcohol, water and mix by 9:3:7, get the upper strata and inject the high speed adverse current chromatogram pipe phase that fixes, take off layer and do moving phase, flow velocity 1ml/min, engine speed 850rpm, moving phase dissolving crude extract, sample introduction, collect flow point according to collection of illustrative plates, preparation continuously, flow point merges concentrate drying, De Maolanfei 1.1g, detect content 97.3% through HPLC.
Claims (2)
1. the preparation method of a hair orchid phenanthrene is characterized in that comprising following steps:
1) with stem of Eyeshaped Dendrobium raw material pulverizing 20-80 order, places CO
2Extract CO in the supercritical extraction jar
2Flow is the 1-5ml/min/g raw material, extraction temperature 30-60 ℃, and pressure 20-30Mpa, extraction time 1-4h, extract dissolves with chloroform, filters, and reclaims reagent and gets crude extract;
2) above-mentioned crude extract is solvent systems with chloroform, methyl alcohol, water, gets the phase that fixes mutually, is mutually moving phase to adopt the high speed adverse current chromatogram purifying down, engine speed 700-1000rpm, flow rate of mobile phase 1-4ml/min collects flow point according to collection of illustrative plates, and the flow point drying under reduced pressure namely.
2. the preparation method of hair orchid phenanthrene as claimed in claim 1 is characterized in that described step 2) in chloroform, methyl alcohol, water for the solvent ratio be: 5-10:2-4:4-9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101944646A CN103265414A (en) | 2013-05-23 | 2013-05-23 | Preparation method of confusarin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101944646A CN103265414A (en) | 2013-05-23 | 2013-05-23 | Preparation method of confusarin |
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| CN103265414A true CN103265414A (en) | 2013-08-28 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2013101944646A Pending CN103265414A (en) | 2013-05-23 | 2013-05-23 | Preparation method of confusarin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105999761A (en) * | 2016-06-27 | 2016-10-12 | 广州纤维产品检测研究院 | Method for rapidly separating polycyclic aromatic hydrocarbons in textiles by using supercritical CO2 fluid |
| 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 |
| CN112870185A (en) * | 2021-02-25 | 2021-06-01 | 沈阳药科大学 | Medicine for treating or preventing cervical cancer of human, preparation method and application |
-
2013
- 2013-05-23 CN CN2013101944646A patent/CN103265414A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105999761A (en) * | 2016-06-27 | 2016-10-12 | 广州纤维产品检测研究院 | Method for rapidly separating polycyclic aromatic hydrocarbons in textiles by using supercritical CO2 fluid |
| CN105999761B (en) * | 2016-06-27 | 2018-11-23 | 广州纤维产品检测研究院 | Using supercritical CO2The method of polycyclic aromatic hydrocarbon in fluid quick separating textile |
| 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 |
| CN112870185A (en) * | 2021-02-25 | 2021-06-01 | 沈阳药科大学 | Medicine for treating or preventing cervical cancer of human, preparation method and application |
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Application publication date: 20130828 |