CN103408403A - Preparation method of rush phenanthrenol - Google Patents
Preparation method of rush phenanthrenol Download PDFInfo
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- CN103408403A CN103408403A CN2013103797001A CN201310379700A CN103408403A CN 103408403 A CN103408403 A CN 103408403A CN 2013103797001 A CN2013103797001 A CN 2013103797001A CN 201310379700 A CN201310379700 A CN 201310379700A CN 103408403 A CN103408403 A CN 103408403A
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- preparation
- rush
- raw material
- drying
- medulla junci
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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 rush phenanthrenol, which is simple and convenient to operate and small in pollution. The preparation method comprises the following steps of drying and crushing a rush raw material into 20-80 meshes; extracting the rush raw material in a supercritical CO2 extraction tank, wherein the flow of CO2 is 1-4ml/min/g of the raw material, the extraction temperature is 30-60 DEG C, the pressure is 15-30Mpa, and the extraction time is 1-4 hours; resolving to obtain an extract, adding neutral aluminum oxide resin, drying and packing; performing elution by sequentially using petroleum ether and acetic ether; collecting an acetic ether eluant, and performing vacuum concentration on the acetic ether eluant; separating the obtained extract by using a high-speed counter-current chromatography; collecting fractions according to a chromatogram; and performing vacuum concentration and drying to obtain the rush phenanthrenol. The preparation method disclosed by the invention is suitable for preparing the rush phenanthrenol.
Description
Technical field
The invention belongs to the Natural Medicine Chemistry field, especially relate to a kind of preparation method of Medulla Junci phenanthrol.
Background technology
The Medulla Junci phenanthrol, molecular formula C17H16O2, molecular weight 252.3, molecular structural formula:
The Medulla Junci phenanthrol be a kind of from Medulla Junci the separate drug chemical composition, have cytotoxic activity.Medulla Junci is stem marrow or the herb of rush family plant Rush, and the stem marrow contains multiple phenanthrene derivatives, has the effect of refrigerant calmness and diuresis.The foreign scholar studies confirm that the sharp-flowered rush plant has very strong antibiotic, anti-oxidant, antitumor and anti-algae activity.
By literature search, the Medulla Junci phenanthrol adopts conventional solvent extraction with silicagel column, to separate preparation, and these class methods exist that yield is low, solvent load is large, with serious pollution technological deficiency.
Summary of the invention
The objective of the invention is to solve prior art deficiency and defect, a kind of preparation method of efficient, oligosaprobic Medulla Junci phenanthrol is provided.
The objective of the invention is to realize by the following technical solutions: a kind of preparation method of Medulla Junci phenanthrol, it is characterized in that: get the Medulla Junci raw material drying and pulverize the 20-80 order, being placed in the SCF-CO 2 tank extracts, the CO2 flow is the 1-4ml/min/g raw material, extraction temperature 30-60 ℃, pressure 15-30Mpa, extraction time 1-4h, resolve to such an extent that extract adds the neutral alumina resin to dry the dress post, use successively sherwood oil, eluent ethyl acetate, collect eluent ethyl acetate liquid concentrating under reduced pressure, gained medicinal extract adopts high-speed countercurrent chromatography to separate again, according to chromatogram, collect flow point, concentrating under reduced pressure is drying to obtain.
Described normal hexane, ethyl acetate, methyl alcohol, water are solvent systems, mix in the 1-4:2-9:3-10:2-7 ratio, get the phase that fixes mutually, be mutually moving phase down.
Adopt present method to prepare the Medulla Junci phenanthrol, extraction efficiency is high, pollutes littlely, and product purity is high, easy handling.
Below in conjunction with embodiment, further illustrate the present invention, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1:
After getting the Medulla Junci raw material drying, pulverize 20 orders, get 2kg, be placed in the SCF-CO 2 tank and extract, passing into the CO2 flow is the 3ml/min/g raw material, 40 ℃ of extraction temperature, pressure 15Mpa, extraction time 2h, gained extract add 100g neutral alumina resin dress post, with 300ml sherwood oil wash-out impurity, use again the 500ml eluent ethyl acetate, collect back segment 400ml elutriant and reclaim reagent, obtain medicinal extract.Getting normal hexane, ethyl acetate, methyl alcohol, water is solvent systems, mixes in the 1:2:3:2 ratio, gets and injects mutually the high speed adverse current chromatogram pipe phase that fixes, take off and do mutually moving phase, flow velocity 2ml/min, engine speed 800rpm, moving phase is dissolved concentrated solution, sample introduction, collect flow point, continuous production according to collection of illustrative plates, flow point merges concentrate drying, obtain Medulla Junci phenanthrol 1.8g, through HPLC, detect content 97.1%.
Embodiment 2:
After getting the Medulla Junci raw material drying, pulverize 40 orders, get 2kg, be placed in the SCF-CO 2 tank and extract, passing into the CO2 flow is the 4ml/min/g raw material, 45 ℃ of extraction temperature, pressure 20Mpa, extraction time 3h, gained extract add 150g neutral alumina resin dress post, with 400ml sherwood oil wash-out impurity, use again the 600ml eluent ethyl acetate, collect back segment 500ml elutriant and reclaim reagent, obtain medicinal extract.Getting normal hexane, ethyl acetate, methyl alcohol, water is solvent systems, mixes in the 2:3:4:5 ratio, gets and injects mutually the high speed adverse current chromatogram pipe phase that fixes, take off and do mutually moving phase, flow velocity 2ml/min, engine speed 850rpm, moving phase is dissolved concentrated solution, sample introduction, collect flow point, continuous production according to collection of illustrative plates, flow point merges concentrate drying, obtain Medulla Junci phenanthrol 1.5g, through HPLC, detect content 97.5%.
Embodiment 3:
After getting the Medulla Junci raw material drying, pulverize 60 orders, get 2kg, be placed in the SCF-CO 2 tank and extract, passing into the CO2 flow is the 2ml/min/g raw material, 50 ℃ of extraction temperature, pressure 25Mpa, extraction time 3h, gained extract add 200g neutral alumina resin dress post, with 400ml sherwood oil wash-out impurity, use again the 600ml eluent ethyl acetate, collect back segment 500ml elutriant and reclaim reagent, obtain medicinal extract.Getting normal hexane, ethyl acetate, methyl alcohol, water is solvent systems, mixes in the 3:7:9:4 ratio, gets and injects mutually the high speed adverse current chromatogram pipe phase that fixes, take off and do mutually moving phase, flow velocity 3ml/min, engine speed 900rpm, moving phase is dissolved concentrated solution, sample introduction, collect flow point, continuous production according to collection of illustrative plates, flow point merges concentrate drying, obtain Medulla Junci phenanthrol 1.9g, through HPLC, detect content 97.3%.
Claims (2)
1. the preparation method of a Medulla Junci phenanthrol, it is characterized in that: get the Medulla Junci raw material drying and pulverize the 20-80 order, being placed in the SCF-CO 2 tank extracts, the CO2 flow is the 1-4ml/min/g raw material, extraction temperature 30-60 ℃, pressure 15-30Mpa, extraction time 1-4h, resolve to such an extent that extract adds the neutral alumina resin to dry the dress post, use successively sherwood oil, eluent ethyl acetate, collect eluent ethyl acetate liquid concentrating under reduced pressure, gained medicinal extract adopts high-speed countercurrent chromatography to separate again, according to chromatogram, collect flow point, concentrating under reduced pressure is drying to obtain.
2. the preparation method of Medulla Junci phenanthrol as claimed in claim 1, is characterized in that described normal hexane, ethyl acetate, methyl alcohol, water are solvent systems, mixes in the 1-4:2-9:3-10:2-7 ratio, gets the phase that fixes mutually, is mutually moving phase down.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013103797001A CN103408403A (en) | 2013-08-28 | 2013-08-28 | Preparation method of rush phenanthrenol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013103797001A CN103408403A (en) | 2013-08-28 | 2013-08-28 | Preparation method of rush phenanthrenol |
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| CN103408403A true CN103408403A (en) | 2013-11-27 |
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| CN2013103797001A Pending CN103408403A (en) | 2013-08-28 | 2013-08-28 | Preparation method of rush phenanthrenol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910110A (en) * | 2015-05-28 | 2015-09-16 | 南京泽朗生物科技有限公司 | Aeginetolide preparation method |
-
2013
- 2013-08-28 CN CN2013103797001A patent/CN103408403A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910110A (en) * | 2015-05-28 | 2015-09-16 | 南京泽朗生物科技有限公司 | Aeginetolide preparation method |
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Application publication date: 20131127 |
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| WD01 | Invention patent application deemed withdrawn after publication |