CN103232503A - Method for preparing verbenalin - Google Patents
Method for preparing verbenalin Download PDFInfo
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- CN103232503A CN103232503A CN 201310183385 CN201310183385A CN103232503A CN 103232503 A CN103232503 A CN 103232503A CN 201310183385 CN201310183385 CN 201310183385 CN 201310183385 A CN201310183385 A CN 201310183385A CN 103232503 A CN103232503 A CN 103232503A
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- ethanolic soln
- verbenaloside
- wash
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- nanofiltration
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- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
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Abstract
The invention discloses a method for preparing verbenalin. The method comprises the following steps of: 1) cutting the verbena raw material into segments, adding decuple water for extraction by heating, adding the extract to an ultrafiltration membrane for ultrafiltration, and then adding the filtrate to a nanofiltration membrane for nanofiltration; collecting a concentrated solution, adding the concentrated solution to an activated charcoal column for absorption, performing gradient elution by using an ethanol solution, and performing decompression concentration on elute until no alcohol exists; and 2) adding the concentrated solution to an alumium oxide resin column for absorption, eluting by using the ethanol solution, concentrating the elute, then performing reflux dissolution of the concentrated elute by using the ethyl acetate solution, and finally, crystallizing in cold storage. The method provided by the invention is simple in production process, high in operability, high in purity of the obtained product, and suitable for industrial production.
Description
Technical field
The invention belongs to biological technical field, particularly a kind of preparation method of verbenaloside.
Background technology
Verbenaloside belongs to iridoid glucosides class material, CAS 548-37-8, molecular formula C
17H
24O
10, molecular weight 388.3, molecular structural formula:
Vervain is herb or the whole herb with root of Verbenaceae plant vervain, belongs to perennial herb, and herb contains verbenaloside, tannin, volatilization wet goods composition, has effects such as clearing heat and detoxicating, promoting blood circulation to remove blood stasis, inducing diuresis to remove edema.Cure mainly fever caused by exogenous pathogens, jaundice due to damp-heat, oedema dysentery, diphtheria larynx numbness, gonorrhoea through close, disease such as miasma lump in the abdomen noma, carbuncle sore tumefacting virus.Verbenaloside is iridoids material in the vervain, has cholagogic, rushes down down and suppress the sympathetic nerve effect.
By literature search, the existing method for preparing verbenaloside from vervain adopts macroporous resin to separate with silicagel column more.This class methods complicated operation, the production cost height.
Summary of the invention
The objective of the invention is to solve prior art deficiency and defective, a kind of preparation method of verbenaloside easy and simple to handle is provided.
The object of the present invention is achieved like this: a kind of preparation method of verbenaloside is characterized in that being following steps:
1) with the segment of vervain raw material, add 10 times of water gaging heating and extract, extracting solution adds the ultra-filtration membrane ultrafiltration, adds the nanofiltration membrane nanofiltration again, collects concentrated solution and adds activated carbon column absorption, and ethanolic soln gradient elution, elutriant are evaporated to does not have alcohol;
2) adsorb in the above-mentioned concentrated solution adding aluminum oxide resin column, the ethanolic soln wash-out, after elutriant concentrated, with ethyl acetate solution backflow dissolving, the refrigeration crystallization was namely.
The hollow composite membrane of the optional molecular weight cut-off 3000-6000 of ultra-filtration membrane in the step 1), nanofiltration membrane are that molecular weight cut-off is 200 hollow composite membrane.
Step 1) ethanolic soln gradient elution is: earlier with 5-10 times of column volume 20-40% ethanolic soln wash-out, use 60-90% ethanolic soln wash-out again.
Step 2) ethanolic soln concentration is the ethanolic soln of 90-95% in the ethanolic soln wash-out, and the wash-out multiple is 7-10 times of column volume.
Adopt the present invention to prepare verbenaloside, production technique is simple, products obtained therefrom purity height, and production cost is low, is easy to realize suitability for industrialized production.
Embodiment:
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 1:
Get the segment of vervain raw material, weighing 10kg, add 10 times of water gagings and be heated to 50 ℃ of immersions 2 hours, extract 3 times, extracting solution merges the hollow composite membrane ultrafiltration that filters adding molecular weight cut-off 3000, see through the hollow composite membrane nanofiltration that liquid adds molecular weight cut-off 200 again, the collection concentrated solution adds to be equipped with in the 500g gac resin column and adsorbs, earlier with 10 times of column volumes, 20% ethanolic soln wash-out, use 8 times of column volumes, 80% ethanolic soln wash-out again, elutriant is evaporated to does not have alcohol, adds to be equipped with in the 300g aluminum oxide resin column and adsorbs 8 times of column volume 90% ethanolic soln wash-outs, elutriant is concentrated into medicinal extract and dissolves with the ethyl acetate solution backflow, filter the refrigeration crystallization, dry white powder 9g, the content 98.6% of getting.
Embodiment 2:
The segment of vervain raw material, weighing 10kg, add 6 times of water gagings and be heated to 60 ℃ of immersions 2 hours, extract 3 times, extracting solution merges the hollow composite membrane ultrafiltration that filters adding molecular weight cut-off 5000, see through the hollow composite membrane nanofiltration that liquid adds molecular weight cut-off 200 again, the collection concentrated solution adds to be equipped with in the 400g gac resin column and adsorbs, earlier with 7 times of column volumes, 30% ethanolic soln wash-out, use 7 times of column volumes, 90% ethanolic soln wash-out again, elutriant is evaporated to does not have alcohol, adds to be equipped with in the 400g aluminum oxide resin column and adsorbs 10 times of column volume 95% ethanolic soln wash-outs, elutriant is concentrated into medicinal extract and dissolves with the ethyl acetate solution backflow, filter the refrigeration crystallization, dry white powder 9.4g, the content 97.7% of getting.
Embodiment 3:
Get the segment of vervain raw material, weighing 10kg, add 7 times of water gagings and be heated to 50 ℃ of immersions 2 hours, extract 3 times, extracting solution merges the hollow composite membrane ultrafiltration that filters adding molecular weight cut-off 6000, see through the hollow composite membrane nanofiltration that liquid adds molecular weight cut-off 200 again, the collection concentrated solution adds to be equipped with in the 500g gac resin column and adsorbs, earlier with 5 times of column volumes, 40% ethanolic soln wash-out, use 6 times of column volumes, 90% ethanolic soln wash-out again, elutriant is evaporated to does not have alcohol, adds to be equipped with in the 300g aluminum oxide resin column and adsorbs 8 times of column volume 95% ethanolic soln wash-outs, elutriant is concentrated into medicinal extract and dissolves with the ethyl acetate solution backflow, filter the refrigeration crystallization, dry white powder 10.3g, the content 98.1% of getting.
Claims (4)
1. the preparation method of a verbenaloside is characterized in that following steps:
1) with the segment of vervain raw material, add 10 times of water gaging heating and extract, extracting solution adds the ultra-filtration membrane ultrafiltration, adds the nanofiltration membrane nanofiltration again, collects concentrated solution and adds activated carbon column absorption, and ethanolic soln gradient elution, elutriant are evaporated to does not have alcohol;
2) adsorb in the above-mentioned concentrated solution adding aluminum oxide resin column, the ethanolic soln wash-out, after elutriant concentrated, with ethyl acetate solution backflow dissolving, the refrigeration crystallization was namely.
2. according to the preparation method of the described verbenaloside of claim 1, it is characterized in that the hollow composite membrane of the optional molecular weight cut-off 3000-6000 of ultra-filtration membrane in the described step 1), nanofiltration membrane is that molecular weight cut-off is 200 hollow composite membrane.
3. according to the preparation method of the described verbenaloside of claim 1, it is characterized in that described step 1) ethanolic soln gradient elution is: earlier with 5-10 times of column volume 20-40% ethanolic soln wash-out, use 60-90% ethanolic soln wash-out again.
4. according to the preparation method of the described verbenaloside of claim 1, it is characterized in that described step 2) ethanolic soln concentration is the ethanolic soln of 90-95% in the ethanolic soln wash-out, the wash-out multiple is 7-10 times of column volume.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310183385 CN103232503A (en) | 2013-05-17 | 2013-05-17 | Method for preparing verbenalin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310183385 CN103232503A (en) | 2013-05-17 | 2013-05-17 | Method for preparing verbenalin |
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| Publication Number | Publication Date |
|---|---|
| CN103232503A true CN103232503A (en) | 2013-08-07 |
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Family Applications (1)
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| CN 201310183385 Pending CN103232503A (en) | 2013-05-17 | 2013-05-17 | Method for preparing verbenalin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111303218A (en) * | 2020-03-17 | 2020-06-19 | 连江仁泽生物科技有限公司 | Synthetic method and application of verbena glycoside |
| CN111423475A (en) * | 2020-03-17 | 2020-07-17 | 连江仁泽生物科技有限公司 | Method for extracting verbena glycoside from verbena and medicine for treating dysmenorrhea |
| CN113329757A (en) * | 2018-11-14 | 2021-08-31 | 芬策尔贝格有限两合公司 | Use of Leptoradix lemonae extract for enhancing neurocerebrum utilization rate of neurotransmitter such as serotonin, dopamine, norepinephrine, etc |
-
2013
- 2013-05-17 CN CN 201310183385 patent/CN103232503A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113329757A (en) * | 2018-11-14 | 2021-08-31 | 芬策尔贝格有限两合公司 | Use of Leptoradix lemonae extract for enhancing neurocerebrum utilization rate of neurotransmitter such as serotonin, dopamine, norepinephrine, etc |
| CN111303218A (en) * | 2020-03-17 | 2020-06-19 | 连江仁泽生物科技有限公司 | Synthetic method and application of verbena glycoside |
| CN111423475A (en) * | 2020-03-17 | 2020-07-17 | 连江仁泽生物科技有限公司 | Method for extracting verbena glycoside from verbena and medicine for treating dysmenorrhea |
| CN111303218B (en) * | 2020-03-17 | 2021-03-30 | 连江仁泽生物科技有限公司 | Synthetic method and application of verbena glycoside |
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Application publication date: 20130807 |