CN101759677A - Preparation method for patchoulenone - Google Patents
Preparation method for patchoulenone Download PDFInfo
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- CN101759677A CN101759677A CN200910232994A CN200910232994A CN101759677A CN 101759677 A CN101759677 A CN 101759677A CN 200910232994 A CN200910232994 A CN 200910232994A CN 200910232994 A CN200910232994 A CN 200910232994A CN 101759677 A CN101759677 A CN 101759677A
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- pogostone
- essential oil
- volatile oil
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a preparation method for patchoulenone. The preparation method is simple to be operated, has lower pollution and little equipment investment. The preparation method comprises the processing steps: taking pogostemon cablin, extracting essential oil until no essential oil is left by steam distillation, separating the essential oil, adding ether, the volume of which is 0.5-2 times of the volume of the essential oil and 1 mol/L of NoOH solution, the volume of which is 1-3 times of the volume of the essential oil, extracting, separating water layers, repeating the operation for 3-8 times, combining the water layers, adding diluted hydrochloric acid and to adjust the pH to be 2-3, laying aside and staying overnight, filtering, taking filter residue, washing until reaching the neutrality, adding normal hexane to dissolve the filter residue, refrigerating and crystallizing. The patchoulenone prepared by the invention has high product purity and easily realizes the industrialization amplification.
Description
Technical field
The present invention relates to a kind of preparation method of pogostone, especially a kind of method of from plant, extracting pogostone.
Background technology
Pogostone (Pogostone), different name: thorn stamen humulone.Molecular formula: C
12H
16O
4, molecular weight: 224.256, CAS accession number: 23800-56-8, structural formula is as follows:
Pogostone is a kind of natural compounds, has physiologically actives such as antibiotic, antiviral, extensively is present in the Labiatae various plants.
The Chinese medicine Wrinkled Gianthyssop Herb is the dry aerial parts of plant Labiatae Wrinkled Gianthyssop Herb Pogostemon cablin (Blanco) Benth., has and eliminates dampness with aromatics, and the appetizing preventing or arresting vomiting is delivered effects such as relieving summer-heat, wherein contains a large amount of pogostones.
In the prior art, the extraction separation of pogostone mainly adopts organic solvent method etc., but the content of the pogostone that these extraction processes obtain is low, and is seriously polluted in the production process, and unfavorable big production operation.
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, pogostone that product purity is high.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
Get Wrinkled Gianthyssop Herb, wet distillation is extracted volatile oil to the greatest extent, separates volatile oil, add the NaOH solution of the 1mol/L that ether that its volume 0.5-2 doubly measures and 1-3 doubly measure, extraction separates water layer, repetitive operation 3-8 time, combining water layer adds dilute hydrochloric acid and regulates pH2-3, placement is spent the night, and filters, and gets filter residue, be washed to neutrality, add n-hexane dissolution, the refrigeration crystallization, fractional crystallization washs, is drying to obtain.
Extraction is preferably 1 times of amount volume of volatile oil volume with the amount of ether.
Extraction is preferably 1.5 times of amount volumes of volatile oil volume with the amount of NaOH solution.
The number of times of extraction is preferably 5 times.
Adopt technique scheme to prepare pogostone, easy and simple to handle, pollute less, equipment drops into for a short time, is beneficial to big production operation.
Below in conjunction with 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 Wrinkled Gianthyssop Herb 10Kg, get Wrinkled Gianthyssop Herb, wet distillation is extracted volatile oil to the greatest extent, separates volatile oil, the NaOH solution that adds the 1mol/L of the ether of 0.5 times of amount of its volume and 1 times of amount, extraction separates water layer, repetitive operation 3 times, combining water layer adds dilute hydrochloric acid and regulates pH2-3, and placement is spent the night, filter, get filter residue, be washed to neutrality, add n-hexane dissolution, refrigeration crystallization, fractional crystallization, wash, be drying to obtain pogostone 4.2g, detect through HPLC, purity is 98.1%.
Embodiment 2
Get Wrinkled Gianthyssop Herb 10Kg, water is got Wrinkled Gianthyssop Herb, and wet distillation is extracted volatile oil to the greatest extent, separates volatile oil, the NaOH solution that adds the 1mol/L of the ether of 2 times of amounts of its volume and 3 times of amounts, extraction separates water layer, repetitive operation 8 times, combining water layer adds dilute hydrochloric acid and regulates pH2-3, and placement is spent the night, filter, get filter residue, be washed to neutrality, add n-hexane dissolution, refrigeration crystallization, fractional crystallization, wash, be drying to obtain pogostone 7.2g, detect through HPLC, purity is 98.0%.
Embodiment 3
Get Wrinkled Gianthyssop Herb 10Kg, wet distillation is extracted volatile oil to the greatest extent, separates volatile oil, adds the NaOH solution of the 1mol/L of the ether of 1 times of amount of its volume and 1.5 times of amounts, extraction separates water layer, repetitive operation 5 times, combining water layer adds dilute hydrochloric acid and regulates pH2-3, and placement is spent the night, filter, get filter residue, be washed to neutrality, add n-hexane dissolution, refrigeration crystallization, fractional crystallization, wash, be drying to obtain pogostone 7.6g, detect through HPLC, purity is 99.6%.
Claims (4)
1. the preparation method of a pogostone is characterized in that described method comprises the following steps: to get Wrinkled Gianthyssop Herb, and wet distillation is extracted volatile oil to most, separate volatile oil, add the NaOH solution of the 1mol/L that ether that its volume 0.5-2 doubly measures and 1-3 doubly measure, extraction, separate water layer, repetitive operation 3-8 time, combining water layer, add dilute hydrochloric acid and regulate pH2-3, placement is spent the night, and filters, get filter residue, be washed to neutrality, add n-hexane dissolution, the refrigeration crystallization, fractional crystallization washs, is drying to obtain.
2. according to the preparation method of the described pogostone of claim 1, it is characterized in that described extraction is 1 times of amount volume of volatile oil volume with the amount of ether.
3. according to the preparation method of the described pogostone of claim 1, it is characterized in that described extraction is 1.5 times of amount volumes of volatile oil volume with the amount of NaOH solution.
4. according to the preparation method of the described pogostone of claim 1, the number of times that it is characterized in that described extraction is 5 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910232994A CN101759677A (en) | 2009-10-20 | 2009-10-20 | Preparation method for patchoulenone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910232994A CN101759677A (en) | 2009-10-20 | 2009-10-20 | Preparation method for patchoulenone |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101759677A true CN101759677A (en) | 2010-06-30 |
Family
ID=42491073
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910232994A Pending CN101759677A (en) | 2009-10-20 | 2009-10-20 | Preparation method for patchoulenone |
Country Status (1)
| Country | Link |
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| CN (1) | CN101759677A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113278597A (en) * | 2021-05-26 | 2021-08-20 | 重庆大学 | Novel short-side-chain fatty acid CoA ligase and application thereof in preparation of patchoulenone |
-
2009
- 2009-10-20 CN CN200910232994A patent/CN101759677A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113278597A (en) * | 2021-05-26 | 2021-08-20 | 重庆大学 | Novel short-side-chain fatty acid CoA ligase and application thereof in preparation of patchoulenone |
| CN113278597B (en) * | 2021-05-26 | 2023-04-21 | 重庆大学 | Novel short side chain fatty acid CoA ligase and application thereof in preparation of patchoulenone |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20100630 |