CN102329321A - Method for extracting citracridone I from citrus depressa hayata root bark - Google Patents
Method for extracting citracridone I from citrus depressa hayata root bark Download PDFInfo
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- CN102329321A CN102329321A CN201110143971A CN201110143971A CN102329321A CN 102329321 A CN102329321 A CN 102329321A CN 201110143971 A CN201110143971 A CN 201110143971A CN 201110143971 A CN201110143971 A CN 201110143971A CN 102329321 A CN102329321 A CN 102329321A
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- China
- Prior art keywords
- extracting
- dihydroketoacridine
- ethanol
- root skin
- citracridone
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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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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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to a method for extracting citracridone I from citrus depressa hayata root bark, which is easy and convenient to operate and has small pollution and low energy consumption. The method comprises the following process steps of: smashing citrus depressa hayata root bark; adding into a CO2 supercritical extractor to obtain an extract by taking ethyl acetate as an entrainer; adding ethanol for dissolving; adding onto a macroporous absorption resin column for adsorbing; eluting with 60-80 percent ethanol; collecting an eluent which is 3-8 times the volume of the column; filtering; recovering ethanol under reduced pressure and concentrating; adding acetone for crystalizing; separating crystals; and washing and drying. Due to the adoption of the method for preparing citracridone I, the product purity is high and industrial amplification is easy to realize.
Description
Technical field
The present invention relates to a kind of preparation method of dihydroketoacridine I, especially a kind of preparation method who from plant, extracts the dihydroketoacridine I.
Background technology
Dihydroketoacridine I (Citracridone I), molecular formula: C20H19NO5, molecular weight: 353.374, CAS accession number: 81525-61-3 mainly is present in the root and root skin of Rutaceae various plants, wherein the flat tangerine of rutaceae
Citrus depressaContent is abundant in the root of Hayata.Its molecular formula is following.
Modern study shows that the dihydroketoacridine I has very strong spasmolysis, and it is also as the raw material that synthesizes other reactive derivative simultaneously.
The flat tangerine of rutaceae
Citrus depressaThe root of Hayata uses as Chinese medicine tangerine root.Effect with promoting the circulation of QI to relieve pain.
In the prior art, still be not applicable to preparation technology's report of high purity dihydroketoacridine I industrialized production.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method who is beneficial to big production operation, dihydroketoacridine I that product purity is high.
For solving the problems of the technologies described above, the present invention adopts following technical proposal.
Get flat tangerine root skin, pulverize, join CO
2In the supercritical extraction device, ETHYLE ACETATE is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 3-7%, extracting pressure 10-30MPa, temperature 30-60 ℃, CO
2Flow 1-3ml/g crude drug min, extraction time 120-180min gets extract; Add dissolve with ethanol, join on the macroporous adsorptive resins and adsorb, the 60-80% ethanol elution; Collect 3-8 and doubly measure the column volume elutriant, filter, decompression recycling ethanol also concentrates; Add the acetone crystallization, fractional crystallization washs, is drying to obtain.
CO
2The volume percent that the supercritical extraction entrainment agent accounts for total extraction solvent is 5%.
CO
2Supercritical extraction pressure 20MPa, 45 ℃ of temperature, CO
2Flow 2ml/g crude drug min, extraction time 150min.
Macroporous adsorbent resin is selected from a kind of in D102 type, AB-8 type, the HPD-700 type macroporous adsorbent resin.
It is 70% that the macroporous adsorbent resin wash-out uses concentration of ethanol, and collecting amount is 5 times of amount column volumes.
Preparation gained dihydroketoacridine I can adopt following method to detect.
Test Example 1 HPLC method is measured dihydroketoacridine I purity
Chromatographic condition
Chromatographic column: octadecylsilane bonding glue silica gel is weighting agent; Moving phase: methyl alcohol-second eyeball (90: 10); Flow velocity: 1mL/min; Detect wavelength: 340nm; Column temperature: 30 ℃.
Measuring method
Precision takes by weighing dihydroketoacridine I 2mg, places the 50mL measuring bottle, adds people's methyl alcohol 20mL, and sonic oscillation makes dissolving, and methanol constant volume is drawn 10 μ L to scale, injects high performance liquid chromatograph, adopts normalization method working sample purity.
Adopt the present invention to prepare the dihydroketoacridine I, be beneficial to big production operation, energy consumption is little, pollutes little.
Below in conjunction with the specific embodiment the present invention is further elaborated, but the scope of protection of present invention is not limited to following embodiment.
Embodiment
Embodiment 1
Get flat tangerine root skin 10Kg, pulverize, join CO
2In the supercritical extraction device, ETHYLE ACETATE is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 3%, extracting pressure 10MPa, 30 ℃ of temperature, CO
2Flow 1ml/g crude drug min, extraction time 120min gets extract, adds dissolve with ethanol; Join on the D102 type macroporous adsorptive resins and adsorb, 60% ethanol elution is collected 3 times of amount column volume elutriants, filters; Decompression recycling ethanol also concentrates, and adds the acetone crystallization, and fractional crystallization washs, is drying to obtain dihydroketoacridine I 11.3g; Detect through HPLC, purity is 94.8%, UV, IR, MS,
2HNMR,
13The data and the prior art of its physical behavior of sign such as CNMR are consistent.
Embodiment 2
Get flat tangerine root skin 10Kg, pulverize, join CO
2In the supercritical extraction device, ETHYLE ACETATE is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 7%, extracting pressure 30MPa, 60 ℃ of temperature, CO
2Flow 3ml/g crude drug min, extraction time 180min gets extract, adds dissolve with ethanol; Join on the HPD-700 type macroporous adsorptive resins and adsorb, 80% ethanol elution is collected 8 times of amount column volume elutriants, filters; Decompression recycling ethanol also concentrates, and adds the acetone crystallization, and fractional crystallization washs, is drying to obtain dihydroketoacridine I 13.2g; Detect through HPLC, purity is 93.3%, UV, IR, MS,
2HNMR,
13The data and the prior art of its physical behavior of sign such as CNMR are consistent.
Embodiment 3
Get flat tangerine root skin 10Kg, pulverize, join CO
2In the supercritical extraction device, ETHYLE ACETATE is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 5%, extracting pressure 20MPa, 45 ℃ of temperature, CO
2Flow 2ml/g crude drug min, extraction time 150min gets extract, adds dissolve with ethanol; Join on the AB-8 type macroporous adsorptive resins and adsorb, 70% ethanol elution is collected 5 times of amount column volume elutriants, filters; Decompression recycling ethanol also concentrates, and adds the acetone crystallization, and fractional crystallization washs, is drying to obtain dihydroketoacridine I 12.6g; Detect through HPLC, purity is 96.1%, UV, IR, MS,
2HNMR,
13The data and the prior art of its physical behavior of sign such as CNMR are consistent.
Claims (5)
1. method of from flat tangerine root skin, extracting the dihydroketoacridine I is characterized in that described method is made up of the following step: get flat tangerine root skin, pulverize, join CO
2In the supercritical extraction device, ETHYLE ACETATE is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 3-7%, extracting pressure 10-30MPa, temperature 30-60 ℃, CO
2Flow 1-3ml/g crude drug min, extraction time 120-180min gets extract; Add dissolve with ethanol, join on the macroporous adsorptive resins and adsorb, the 60-80% ethanol elution; Collect 3-8 and doubly measure the column volume elutriant, filter, decompression recycling ethanol also concentrates; Add the acetone crystallization, fractional crystallization washs, is drying to obtain.
2. according to the said method of from flat tangerine root skin, extracting the dihydroketoacridine I of claim 1, it is characterized in that said CO
2The volume percent that the supercritical extraction entrainment agent accounts for total extraction solvent is 5%.
3. according to the said method of from flat tangerine root skin, extracting the dihydroketoacridine I of claim 1, it is characterized in that said CO
2Supercritical extraction pressure 20MPa, 45 ℃ of temperature, CO
2Flow 2ml/g crude drug min, extraction time 150min.
4. according to the said method of from flat tangerine root skin, extracting the dihydroketoacridine I of claim 1, it is characterized in that said macroporous adsorbent resin is selected from a kind of in D102 type, AB-8 type, the HPD-700 type macroporous adsorbent resin.
5. according to the said method of from flat tangerine root skin, extracting the dihydroketoacridine I of claim 1, it is characterized in that it is 70% that said macroporous adsorbent resin wash-out uses concentration of ethanol, collecting amount is 5 times of amount column volumes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110143971A CN102329321A (en) | 2011-05-31 | 2011-05-31 | Method for extracting citracridone I from citrus depressa hayata root bark |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110143971A CN102329321A (en) | 2011-05-31 | 2011-05-31 | Method for extracting citracridone I from citrus depressa hayata root bark |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102329321A true CN102329321A (en) | 2012-01-25 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110143971A Pending CN102329321A (en) | 2011-05-31 | 2011-05-31 | Method for extracting citracridone I from citrus depressa hayata root bark |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102329321A (en) |
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2011
- 2011-05-31 CN CN201110143971A patent/CN102329321A/en active Pending
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120125 |