CN103275134A - Method for extracting phyllanthus niruri glycoside from phyllanthus niruri - Google Patents
Method for extracting phyllanthus niruri glycoside from phyllanthus niruri Download PDFInfo
- Publication number
- CN103275134A CN103275134A CN 201310194380 CN201310194380A CN103275134A CN 103275134 A CN103275134 A CN 103275134A CN 201310194380 CN201310194380 CN 201310194380 CN 201310194380 A CN201310194380 A CN 201310194380A CN 103275134 A CN103275134 A CN 103275134A
- Authority
- CN
- China
- Prior art keywords
- methanol solution
- herba scopariae
- phyllanthus niruri
- extract
- glycosides
- 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
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for extracting phyllanthus niruri glycoside from phyllanthus niruri. The method is simple in operation and low in pollution and comprises the following steps of: (1) crushing medicinal phyllanthus niruri materials, adding 80-90% methanol solution which is 5-10 times that of the crushed medicinal phyllanthus niruri materials in volume, carrying out ultrasonic extraction for 2-3 times, concentrating extract, adding water to the concentrated extract so as to disperse the concentrated extract, filtering, adding filtrate in macroporous resin so as to carry out adsorption, carrying out gradient elution by using a methanol solution, and concentrating eluate so as to obtain concentrate; and (2) extracting the concentrate for 2-3 times by using a n-butanol solution, recovering n-butanol from extract, then diluting the extract by using water, adding the diluted extract into an ODS (Oxide Dispersion Strengthened) column for adsorption, eluting by using a 30% methanol solution, carrying out thin-layer detection, collecting fractions, and drying under reduced pressure, thereby obtaining the phyllanthus niruri glycoside. By adopting the method for extracting the phyllanthus niruri glycoside, the purity of the obtained product is high, and the industrialized amplification is easy to realize.
Description
Technical field
The invention belongs to the Natural Medicine Chemistry field, relate to a kind of from Herba Scopariae the method for purification Herba Scopariae glycosides.
Background technology
Herba Scopariae is Euphorbiaceae (Euphorbiaceae) plant Herba Scopariae
Phyllanthus niruriL is a kind of widely distributed medicinal plant, hepatitis and the urinary stone disease of being used for the treatment of among the people.Modern study is found, contains type compounds such as flavonoid, phenylpropyl alcohol chlorins compound in the Herba Scopariae, have antiviral, protect the liver, angiotensin-converting enzyme suppresses and effect such as immunosuppression.
The Herba Scopariae glycosides is the plain glycoside material of the phenylpropyl alcohol in the Herba Scopariae, white amorphous powder, and molecular formula is C
38H
42O
17, molecular weight is 770.74, molecular structural formula is:
Modern pharmacological research shows that the Herba Scopariae glycosides has anti-HIV effect, suppress to be denoted as [
33P] combination of RRE (REV-responsive element) RNA and HIV-REV (regulation of virion expression) albumen, its IC
50Being 3.3 μ M, is special HIV-REV albumen/RRE RNA inhibitor.
By literature search, the method for purification Herba Scopariae glycosides discloses less from Herba Scopariae.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of method of easy and simple to handle, product purity is high from Herba Scopariae purification Herba Scopariae glycosides.
For achieving the above object, the present invention is by the following technical solutions:
A kind of from Herba Scopariae the method for purification Herba Scopariae glycosides, it is characterized in that may further comprise the steps:
1) get the Herba Scopariae pulverizing medicinal materials, add 5-10 and doubly measure 80-90% methanol solution supersound extraction 2-3 time, extracting solution concentrates and adds water-dispersion, filters, add in the macroporous resin again and adsorb, the methanol solution gradient elution, elutriant concentrated concentrated solution;
2) above-mentioned concentrated solution extracts 2-3 time with butanol solution, and dilute with water behind the extraction liquid recovery propyl carbinol adds in the ODS post and adsorbs, 30% methanol solution wash-out, and thin layer detects, and collects the flow point drying under reduced pressure and namely gets the Herba Scopariae glycosides.
Described macroporous resin model is: AB-8, ADS-21, HZ-818, NK-9.
Described methanol solution gradient elution is: 3-5 times of column volume 10-30% methanol solution wash-out impurity, 4-6 times of column volume 40-70% methanol solution wash-out effective constituent.
Adopt present method purification Herba Scopariae glycosides, technology is simple to operation, pollute little, products obtained therefrom purity height.
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:
Embodiment 1:
Herba Scopariae 5kg pulverizes, and gets the extractor jar, adds 50kg80% methanol solution supersound extraction 30 minutes, extract 2 times, the united extraction concentrating under reduced pressure adds behind the concentrated solution dilute with water in the 3L AB-8 macroporous resin column and adsorbs, flow velocity 20ml/min, behind the last sample, with 10L 10% methanol solution wash-out impurity, use 15L50% methanol solution wash-out effective constituent again, collect the elutriant concentrating under reduced pressure, get concentrated solution 800ml, add the extraction of 1600ml butanol solution, extract 2 times, the extraction liquid concentrating under reduced pressure, the concentrated solution dilute with water adds to be equipped with in the 100gODS resin column and adsorbs flow rate control 3ml/min, end of the sample, get 30% methanol solution wash-out, thin layer detects, the Fractional Collections flow point, with high density flow point concentrating under reduced pressure drying, get Herba Scopariae glycosides 3.1g, detect content 98.5% through HPLC.
Embodiment 2:
Herba Scopariae 5kg pulverizes, and gets the extractor jar, adds 30kg80% methanol solution supersound extraction 30 minutes, extract 3 times, the united extraction concentrating under reduced pressure adds behind the concentrated solution dilute with water in the 3L ADS-21 macroporous resin column and adsorbs, flow velocity 30ml/min, behind the last sample, with 12L 20% methanol solution wash-out impurity, use 15L60% methanol solution wash-out effective constituent again, collect the elutriant concentrating under reduced pressure, get concentrated solution 700ml, add the extraction of 1000ml butanol solution, extract 3 times, the extraction liquid concentrating under reduced pressure, the concentrated solution dilute with water adds to be equipped with in the 100gODS resin column and adsorbs flow rate control 2ml/min, end of the sample, get 30% methanol solution wash-out, thin layer detects, the Fractional Collections flow point, with high density flow point concentrating under reduced pressure drying, get Herba Scopariae glycosides 3.8g, detect content 98.8% through HPLC.
Embodiment 3:
Herba Scopariae 5kg pulverizes, and gets the extractor jar, adds 50kg90% methanol solution supersound extraction 30 minutes, extract 2 times, the united extraction concentrating under reduced pressure adds behind the concentrated solution dilute with water in the 3L HZ-818 macroporous resin column and adsorbs, flow velocity 20ml/min, behind the last sample, with 10L30% methanol solution wash-out impurity, use 12L60% methanol solution wash-out effective constituent again, collect the elutriant concentrating under reduced pressure, get concentrated solution 600ml, add the extraction of 900ml butanol solution, extract 3 times, the extraction liquid concentrating under reduced pressure, the concentrated solution dilute with water adds to be equipped with in the 100gODS resin column and adsorbs flow rate control 3ml/min, end of the sample, get 30% methanol solution wash-out, thin layer detects, the Fractional Collections flow point, with high density flow point concentrating under reduced pressure drying, get Herba Scopariae glycosides 3.9g, detect content 97.1% through HPLC.
Embodiment 4:
Herba Scopariae 5kg pulverizes, and gets the extractor jar, adds 25kg90% methanol solution supersound extraction 30 minutes, extract 3 times, the united extraction concentrating under reduced pressure adds behind the concentrated solution dilute with water in the 3L NK-9 macroporous resin column and adsorbs, flow velocity 25ml/min, behind the last sample, with 10L 30% methanol solution wash-out impurity, use 20L50% methanol solution wash-out effective constituent again, collect the elutriant concentrating under reduced pressure, get concentrated solution 1000ml, add the extraction of 2000ml butanol solution, extract 2 times, the extraction liquid concentrating under reduced pressure, the concentrated solution dilute with water adds to be equipped with in the 100gODS resin column and adsorbs flow rate control 2ml/min, end of the sample, get 30% methanol solution wash-out, thin layer detects, the Fractional Collections flow point, with high density flow point concentrating under reduced pressure drying, get Herba Scopariae glycosides 4.1g, detect content 98.1% through HPLC.
Claims (3)
1. the method for a purification Herba Scopariae glycosides from Herba Scopariae is characterized in that may further comprise the steps:
1) get the Herba Scopariae pulverizing medicinal materials, add 5-10 and doubly measure 80-90% methanol solution supersound extraction 2-3 time, extracting solution concentrates and adds water-dispersion, filters, add in the macroporous resin again and adsorb, the methanol solution gradient elution, elutriant concentrated concentrated solution;
2) above-mentioned concentrated solution extracts 2-3 time with butanol solution, and dilute with water behind the extraction liquid recovery propyl carbinol adds in the ODS post and adsorbs, 30% methanol solution wash-out, and thin layer detects, and collects the flow point drying under reduced pressure and namely gets the Herba Scopariae glycosides.
As claimed in claim 1 from Herba Scopariae the method for purification Herba Scopariae glycosides, it is characterized in that the macroporous resin model described in the step 1) is: AB-8, ADS-21, HZ-818, NK-9.
As claimed in claim 1 from Herba Scopariae the method for purification Herba Scopariae glycosides, it is characterized in that the gradient elution of methanol solution described in the step 1) is: 3-5 times of column volume 10-30% methanol solution wash-out impurity, 4-6 times of column volume 40-70% methanol solution wash-out effective constituent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310194380 CN103275134A (en) | 2013-05-23 | 2013-05-23 | Method for extracting phyllanthus niruri glycoside from phyllanthus niruri |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310194380 CN103275134A (en) | 2013-05-23 | 2013-05-23 | Method for extracting phyllanthus niruri glycoside from phyllanthus niruri |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103275134A true CN103275134A (en) | 2013-09-04 |
Family
ID=49057777
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201310194380 Pending CN103275134A (en) | 2013-05-23 | 2013-05-23 | Method for extracting phyllanthus niruri glycoside from phyllanthus niruri |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103275134A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106333988A (en) * | 2016-09-30 | 2017-01-18 | 安徽华澳生物技术有限公司 | Preparation method and application of bitter phyllanchus amarus extract |
-
2013
- 2013-05-23 CN CN 201310194380 patent/CN103275134A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106333988A (en) * | 2016-09-30 | 2017-01-18 | 安徽华澳生物技术有限公司 | Preparation method and application of bitter phyllanchus amarus extract |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102276679B (en) | Method for extracting high-purity tea saponin from oil-tea-cake by decompression boiling | |
| CN101130548A (en) | Method for extracting and producing high content arteannuin | |
| CN102617468A (en) | Method for ultrasound-assisted extraction of lappaconitine | |
| CN103214533A (en) | Method for continuously preparing cordycepin and cordyceps polysaccharide by using membrane separation technology | |
| CN103694364A (en) | Method for synchronously extracting, separating and purifying polysaccharides and flavones of cyclocarya paliurus | |
| CN101168537A (en) | Method for simultaneously preparing andrographolide and dehydrated andrographolide | |
| CN101525328B (en) | Method for extracting alpha-mangostin from mangosteen fruit peel | |
| CN103408610A (en) | Method for extracting arbutin from pear leaves | |
| CN103265554A (en) | Preparation method of demethylwedelolactone | |
| CN107298687A (en) | Purification maackiain technique is extracted from beautiful millettia root | |
| CN103265521A (en) | Preparation method of demethylated beilidifolin | |
| CN103275134A (en) | Method for extracting phyllanthus niruri glycoside from phyllanthus niruri | |
| CN108997359A (en) | A method of chlorophyll is extracted from stevioside production waste residue | |
| CN106986904A (en) | A kind of Gastrodin extracted in the anesthesia stem from day and preparation method thereof | |
| CN103408615A (en) | Preparation method for chemical reference substance of sweroside in Tibetan capillary artemisia medicinal material | |
| CN104473981B (en) | A kind of isolation and purification method of high-purity autumn eggplant leaf flavonoids | |
| CN104072570A (en) | Preparation method of momordin Ic | |
| CN102250183A (en) | Method for preparing high-purity ginsenoside Re by using ginseng flower buds as raw materials | |
| CN104711312B (en) | The method that Astragaloside IV is prepared using Trichoderma viride | |
| CN106943442B (en) | Antiviral traditional Chinese medicine extract and preparation method thereof | |
| CN101879265A (en) | Process for co-producing total saponins and polysaccharide from star-of-Bethlehem | |
| CN103275144A (en) | Method for preparing acteoside from rehmannia leaves | |
| CN103450315A (en) | Preparation method of sliver-white aglaione A | |
| CN103739649A (en) | Preparation method for mussaendoside G | |
| CN103709213B (en) | A kind of processing method of extraction purification TSG from Tuber Fleeceflower Root |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130904 |