CN101812113A - Method for preparing ardisia pusilla saponin I - Google Patents
Method for preparing ardisia pusilla saponin I Download PDFInfo
- Publication number
- CN101812113A CN101812113A CN201010170596A CN201010170596A CN101812113A CN 101812113 A CN101812113 A CN 101812113A CN 201010170596 A CN201010170596 A CN 201010170596A CN 201010170596 A CN201010170596 A CN 201010170596A CN 101812113 A CN101812113 A CN 101812113A
- Authority
- CN
- China
- Prior art keywords
- ardisia pusilla
- extraction
- saponin
- ardisia
- preparation
- 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.)
- Pending
Links
Landscapes
- Steroid Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a method for preparing ardisia pusilla saponin I, which has the advantages of simple operation, little pollution and low energy consumption. The method comprises the following steps of: crushing whole plants of ardisia pusilla, adding water in a volume 4 to 8 times the mass of the ardisia pusilla, and putting the mixture in a microwave extraction device to perform microwave extraction at an extraction power of 300 to 600W for 5 to 10 minutes for 2 to 4 times; mixing all extraction solution, filtering the mixed solution and condensing the filtrate, adding water saturated normal butyl alcohol, of which the volume is the same as that of the extraction solution, into the condense to perform extraction for 3 to 8 times, picking up the normal butyl alcohol layers, mixing all normal butyl alcohol layers, filtering the normal butyl alcohol layers, and completely recovering the normal butyl alcohol under vacuum; and adding the obtained extract on a D101 macroporous absorption resin column for adsorption, eluting the extract by using 30 to 50 percent ethanol, collecting eluent, of which the volume is 3 to 8 times that of the solution, filtering the eluent, recovering ethanol under vacuum, condensing the filtrate, adding methanol for crystallization, separating the crystals and drying the crystals to obtain the ardisia pusilla saponin I. The ardisia pusilla saponin I prepared by the method has the advantages of high product purity and easy realization of industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method of ardisia pusilla saponin I, especially a kind of preparation method who from plant, extracts ardisia pusilla saponin I.
Background technology
Ardisia pusilla saponin I (Ardipusilloside I), molecular formula: C
53H
86O
22, molecular weight: 1075.249, CAS accession number: 153127-34-5 mainly is present among the Myrsinacea plant Ardisia pusilla Ardisia pusilla A.DC..Its molecular formula is as follows:
Modern study shows, antitumor, strengthening immunity effect that ardisia pusilla saponin I has.
In the prior art, still be not applicable to preparation technology's report of ardisia pusilla saponin 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, ardisia pusilla saponin I that product purity is high.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
Get the Ardisia pusilla complete stool, pulverize, add the water that its quality 4-8 doubly measures volume, drop in the microwave extracting apparatus and carry out microwave extracting, extraction power 300-600W extracts 2-4 time, each 5-10 minute, combining extraction liquid filters, and concentrates, add equal-volume water-saturated n-butanol extraction 3-8 time, get n-butanol layer, merge, filter, the reclaim under reduced pressure propyl carbinol is to most, join on the D101 macroporous adsorptive resins and adsorb, the 30-50% ethanol elution is collected 3-8 and is doubly measured elutriant, filter, decompression recycling ethanol also concentrates, and adds methanol crystallization, separates, is drying to obtain.
The microwave extracting water consumption is preferably 6 times of amounts of quality of medicinal material volume.
The preferred power 500W of microwave extracting extracts each 8 minutes 3 times.
The water-saturated n-butanol extraction times is preferably 5 times.
Wash-out is preferably 40% with concentration of ethanol.
The collecting amount of elutriant is preferably 5 times of amount column volumes.
Adopt the present invention to prepare ardisia pusilla saponin I, be beneficial to big production operation, energy consumption is little, pollutes little.
The present invention is further elaborated below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment
Embodiment 1
Get Ardisia pusilla complete stool 10Kg, pulverize, add the water of 4 times of amounts of its quality volume, drop in the microwave extracting apparatus and carry out microwave extracting, extraction power 300W extracts 2 times, each 5 minutes, combining extraction liquid filtered, concentrate, add equal-volume water-saturated n-butanol extraction 3 times, get n-butanol layer, merge, filter, the reclaim under reduced pressure propyl carbinol joins on the D101 macroporous adsorptive resins and adsorbs to the greatest extent, 30% ethanol elution, collect 3 times of amount elutriants, filter, decompression recycling ethanol also concentrates, add methanol crystallization, separate, be drying to obtain ardisia pusilla saponin I 8.7g, detect through HPLC, purity is 98.7%.
Embodiment 2
Get Ardisia pusilla complete stool 10Kg, pulverize, add the water of 8 times of amounts of its quality volume, drop in the microwave extracting apparatus and carry out microwave extracting, extraction power 600W extracts 4 times, each 10 minutes, combining extraction liquid filtered, concentrate, add equal-volume water-saturated n-butanol extraction 8 times, get n-butanol layer, merge, filter, the reclaim under reduced pressure propyl carbinol joins on the D101 macroporous adsorptive resins and adsorbs to the greatest extent, 50% ethanol elution, collect 8 times of amount elutriants, filter, decompression recycling ethanol also concentrates, add methanol crystallization, separate, be drying to obtain ardisia pusilla saponin I 12.3g, detect through HPLC, purity is 98.0%.
Embodiment 3
Get Ardisia pusilla complete stool 10Kg, pulverize, add the water of 6 times of amounts of its quality volume, drop in the microwave extracting apparatus and carry out microwave extracting, extraction power 500W extracts 3 times, each 8 minutes, combining extraction liquid filtered, concentrate, add equal-volume water-saturated n-butanol extraction 5 times, get n-butanol layer, merge, filter, the reclaim under reduced pressure propyl carbinol joins on the D101 macroporous adsorptive resins and adsorbs to the greatest extent, 40% ethanol elution, collect 5 times of amount elutriants, filter, decompression recycling ethanol also concentrates, add methanol crystallization, separate, be drying to obtain ardisia pusilla saponin I 11.2g, detect through HPLC, purity is 99.2%.
Claims (6)
1. the preparation method of an ardisia pusilla saponin I is characterized in that described method is made up of the following step: get the Ardisia pusilla complete stool, pulverize, add its quality 4-8 and doubly measure the water of volume, drop in the microwave extracting apparatus and carry out microwave extracting, extraction power 300-600W, extract 2-4 time, each 5-10 minute, combining extraction liquid, filter, concentrate, add equal-volume water-saturated n-butanol extraction 3-8 time, get n-butanol layer, merge, filter, the reclaim under reduced pressure propyl carbinol joins on the D101 macroporous adsorptive resins and adsorbs to the greatest extent, the 30-50% ethanol elution, collect 3-8 and doubly measure elutriant, filter, decompression recycling ethanol also concentrates, add methanol crystallization, separate, be drying to obtain.
2. according to the preparation method of the described a kind of ardisia pusilla saponin I of claim 1, it is characterized in that described microwave extracting water consumption is 6 times of amounts of quality of medicinal material volume.
3. according to the preparation method of the described a kind of ardisia pusilla saponin I of claim 1, it is characterized in that described microwave extracting power 500W, extract each 8 minutes 3 times.
4. according to the preparation method of the described a kind of ardisia pusilla saponin I of claim 1, it is characterized in that described water-saturated n-butanol extraction times is 5 times.
5. according to the preparation method of the described a kind of ardisia pusilla saponin I of claim 1, it is characterized in that described wash-out concentration of ethanol is 40%.
6. according to the preparation method of the described a kind of ardisia pusilla saponin I of claim 1, the collecting amount that it is characterized in that described elutriant is 5 times of amount column volumes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010170596A CN101812113A (en) | 2010-05-13 | 2010-05-13 | Method for preparing ardisia pusilla saponin I |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010170596A CN101812113A (en) | 2010-05-13 | 2010-05-13 | Method for preparing ardisia pusilla saponin I |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101812113A true CN101812113A (en) | 2010-08-25 |
Family
ID=42619492
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010170596A Pending CN101812113A (en) | 2010-05-13 | 2010-05-13 | Method for preparing ardisia pusilla saponin I |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101812113A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102228574A (en) * | 2011-06-30 | 2011-11-02 | 贵阳中医学院 | Preparation method of root of Japanese banana extract and product and application thereof |
| CN102603860A (en) * | 2011-01-25 | 2012-07-25 | 苏州宝泽堂医药科技有限公司 | Method for purifying ardipusilloside I |
-
2010
- 2010-05-13 CN CN201010170596A patent/CN101812113A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603860A (en) * | 2011-01-25 | 2012-07-25 | 苏州宝泽堂医药科技有限公司 | Method for purifying ardipusilloside I |
| CN102228574A (en) * | 2011-06-30 | 2011-11-02 | 贵阳中医学院 | Preparation method of root of Japanese banana extract and product and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102276679A (en) | Method for extracting high-purity tea saponin from oil-tea-cake by decompression boiling | |
| CN104306428B (en) | A method of the extraction purification gypenoside from gynostemma pentaphylla | |
| CN101759757A (en) | Preparation method of glycyrrhizic acid | |
| CN101812113A (en) | Method for preparing ardisia pusilla saponin I | |
| CN104189073B (en) | The preparation method of salvianolic acid | |
| CN102180934A (en) | Preparation method of tubeimoside I | |
| CN101817832A (en) | Method for preparing sikimin | |
| CN103739648A (en) | Preparation method for mussaendoside U | |
| CN102329346A (en) | Method for extracting echinacoside from cistanche deserticola | |
| CN107721857A (en) | A kind of method that high-purity chlorogenic acid is prepared from Gynura procumbens (Lour.) Merr | |
| CN103110689A (en) | Novel method for extracting astragaloside from radix astragali | |
| CN102911218B (en) | Method for synchronously separating liquiritin and liquiritin apioside from liquorice | |
| CN102030758A (en) | Preparation method of chalepensin | |
| CN101955487A (en) | Method for preparing Morusin | |
| CN101759734A (en) | Method for preparing arctiin | |
| CN102250169A (en) | Preparation method for frangulin B | |
| CN102060828B (en) | Preparation method of broussin | |
| CN103739649A (en) | Preparation method for mussaendoside G | |
| CN102763687B (en) | Method for gathering and purifying general flavone from Helianthus tuberosus L. leaves by adopting macroporous resin | |
| CN101830960A (en) | Method for preparing celastrine | |
| CN102010449A (en) | Method for preparing geraniin | |
| CN102020682A (en) | Preparation method of neuchebulagicacid | |
| CN102268049A (en) | Method for extracting cyanogenic glycoside from Rhodiola henryi | |
| CN102010401A (en) | Method for preparing diphyllin | |
| CN103421071A (en) | Preparation method of high-purity ganodermanontriol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| 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: 20100825 |