CN109111452A - The preparation method of adhatodine - Google Patents
The preparation method of adhatodine Download PDFInfo
- Publication number
- CN109111452A CN109111452A CN201810733384.6A CN201810733384A CN109111452A CN 109111452 A CN109111452 A CN 109111452A CN 201810733384 A CN201810733384 A CN 201810733384A CN 109111452 A CN109111452 A CN 109111452A
- Authority
- CN
- China
- Prior art keywords
- adhatodine
- preparation
- extraction
- organic solvent
- concentrate
- Prior art date
- 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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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D487/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00
- C07D487/02—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00 in which the condensed system contains two hetero rings
- C07D487/04—Ortho-condensed systems
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Nitrogen Condensed Heterocyclic Rings (AREA)
Abstract
A kind of preparation method for extraction adhatodine that the present invention designs specifically comprises the following steps: that (1) is packed into the seed drying of Chinese medicine harmel, crushing in extraction vessel；(2) it uses organic solvent refluxing extraction 2-4 times, combined extract, recycle organic solvent and is concentrated into appropriate；(3) SEPHADEX LH-20 is used to separate as separating medium to concentrate；(4) concentrate freezing and crystallizing is gone out into adhatodine.The preparation method of the obtained adhatodine of the present invention, simple process not only environmental protection but also had reduced costs.The method is easy simultaneously is quickly separated using SEPHADEX LH-20, and purity is high is high-quality, has reached good effect.
Description
Technical field
The present invention relates to a kind of extraction preparation methods of medium-height grass explosive component, the especially preparation method of adhatodine.
Background technique
Peganum Three Plants are the monoids of most original in zygophyllaceae, share six kinds, are distributed in the ground such as Asia, Europe, north African,
There are three types of China, i.e., harmel, camel wormwood artemisia split silver more, are distributed mainly on the desertes such as the new northwestward, illiteracy, Shan, sweet, peaceful, half famine
Unconcerned area, resource very abundant.In the prior art, adhatodine is extracted by the seed of harmel, extracts the work of adhatodine
Skill is complicated, loss of effective components is big, and extraction yield is lower, higher cost, and largely wastes Chinese material medicine resource.
Summary of the invention
To solve the above problems, the invention proposes a kind of environmental protection and low-cost preparation extraction adhatodine sides
Method.
A kind of preparation method for extraction adhatodine that the present invention designs, specifically comprises the following steps:
(1) it by the seed drying of Chinese medicine harmel, crushing, is packed into extraction vessel；
(2) it uses organic solvent refluxing extraction 2-4 times, combined extract, recycle organic solvent and is concentrated into appropriate；
(3) SEPHADEX LH-20 is used to separate as separating medium to concentrate；
(4) concentrate freezing and crystallizing is gone out into adhatodine.
Preferably, the organic solvent of extraction can be ethyl alcohol, acetone, petroleum ether, ether；
Preferably, the number of the extraction of reflux is 2 times；
Compared with prior art, the preparation method of the obtained adhatodine of the present invention, simple process not only environmental protection but also had been reduced into
This.The method is easy simultaneously is quickly separated using SEPHADEX LH-20, and purity is high is high-quality, has reached good effect
Fruit.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention.
Embodiment 1
A kind of preparation method of adhatodine, specifically comprises the following steps: designed by the present invention
(1) it by the seed drying of Chinese medicine harmel, crushing, is packed into extraction vessel；
(2) it is extracted 2 times, combined extract, recycle ethyl alcohol and is concentrated into appropriate with alcohol reflux；
(3) SEPHADEX LH-20 is used to separate as separating medium to concentrate；
(4) concentrate freezing and crystallizing is gone out into adhatodine.
Embodiment 2
A kind of preparation method of adhatodine, specifically comprises the following steps: designed by the present invention
(1) it by the seed drying of Chinese medicine harmel, crushing, is packed into extraction vessel；
(2) it is extracted 2 times, combined extract, recycle acetone and is concentrated into appropriate with acetone reflux；
(3) SEPHADEX LH-20 is used to separate as separating medium to concentrate；
(4) concentrate freezing and crystallizing is gone out into adhatodine.
Embodiment 3
A kind of preparation method of adhatodine, specifically comprises the following steps: designed by the present invention
(1) it by the seed drying of Chinese medicine harmel, crushing, is packed into extraction vessel；
(2) it is extracted 2 times, combined extract, recycle ether and is concentrated into appropriate with aether backflow；
(3) SEPHADEX LH-20 is used to separate as separating medium to concentrate；
(4) concentrate freezing and crystallizing is gone out into adhatodine.
Claims (3)
1. a kind of preparation method of adhatodine, it is characterised in that preparation method specifically comprises the following steps:
(1) Chinese medicine being herded horses, grass is dry, crushes, and is packed into extraction vessel；
(2) it uses organic solvent refluxing extraction 2-4 times, combined extract, recycle organic solvent and is concentrated into appropriate；
(3) acidic aqueous solution is adjusted to certain pH value；
(4) concentrate freezing and crystallizing is gone out into thermopsine.
2. a kind of preparation method of adhatodine according to claim 1, it is characterised in that: extraction in step (1)
Organic solvent can be ethyl alcohol, acetone, petroleum ether, ether；
A kind of preparation method of adhatodine according to claim 1, it is characterised in that: refluxing extraction in step (2)
Number is 2 times.
3. the preparation method of adhatodine according to claim 1, it is characterised in that: step (3) will be concentrated with dilute hydrochloric acid
Liquid is deployed into PH=2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810733384.6A CN109111452A (en) | 2018-07-06 | 2018-07-06 | The preparation method of adhatodine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810733384.6A CN109111452A (en) | 2018-07-06 | 2018-07-06 | The preparation method of adhatodine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109111452A true CN109111452A (en) | 2019-01-01 |
Family
ID=64822902
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810733384.6A Withdrawn CN109111452A (en) | 2018-07-06 | 2018-07-06 | The preparation method of adhatodine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109111452A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101433565A (en) * | 2008-11-26 | 2009-05-20 | 上海中医药大学 | Total alkaloid extract of seeds of harmel genus and effective monomer component thereof, and preparation and use thereof |
-
2018
- 2018-07-06 CN CN201810733384.6A patent/CN109111452A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101433565A (en) * | 2008-11-26 | 2009-05-20 | 上海中医药大学 | Total alkaloid extract of seeds of harmel genus and effective monomer component thereof, and preparation and use thereof |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20190101 |