CN101249132A - Preparation technique of humifuse euphorbia effective ingredient - Google Patents
Preparation technique of humifuse euphorbia effective ingredient Download PDFInfo
- Publication number
- CN101249132A CN101249132A CNA200810103792XA CN200810103792A CN101249132A CN 101249132 A CN101249132 A CN 101249132A CN A200810103792X A CNA200810103792X A CN A200810103792XA CN 200810103792 A CN200810103792 A CN 200810103792A CN 101249132 A CN101249132 A CN 101249132A
- Authority
- CN
- China
- Prior art keywords
- extract
- herba euphorbiae
- euphorbiae humifusae
- ethanol
- 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
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to a preparation method of the active ingredient of humifuse euphorbia. After being extracted through menstruum, humifuse euphorbia medicinal material is absorbed and combined by adopting alkali extraction and acid precipitation and polyamide resin to prepare the active ingredient thereof, the active ingredient of the obtained extract has high content, and the process operation is simple and feasible.
Description
Technical field
The invention belongs to natural drug effective ingredient preparation field, be specifically related to a kind of preparation technology of Herba Euphorbiae Humifusae effective ingredient.
Background technology
Herba Euphorbiae Humifusae is the ground herb of Euphorbiaceae euphorbia Herba Euphorbiae Humifusae (Euphorbia himifusa Willd.), has another name called Herba Chenopodii Hybridi, red shank grass, Herba euphorbiae prostratae, milk grass etc., is born in wasteland, open country, roadside, field, and aboundresources is distributed more widely.Herba Euphorbiae Humifusae belongs to antipyretic and antidotal type Chinese medicine, effect with heat-clearing and toxic substances removing, promoting blood circulation and hemostasis, dampness removing lactogenesis, be usually used in treatment and let out dysentery, too fat to move furuncle, hemorrhage, jaundice due to damp-heat and galactostasis etc., be widely used in clinically, its water decoction, tincture have better curative effect to bacillary dysentery, enteritis etc.Its composition mainly contains flavonoid and tannin class, and the tannin composition is more in its middle period.At present, the Herba Euphorbiae Humifusae corresponding preparation is similar to the ubiquitous problem of Chinese medicine compound preparation, and promptly dose is bigger.Chinese patent CN1895331A discloses Herba Euphorbiae Humifusae effective site and the purposes of effective ingredient in the medicine of preparation antifungic action thereof, the effective site of its gained is that the simple decocting of Herba Euphorbiae Humifusae medical material warp boils or ethanol simply extracts, or handle through macroporous absorption at most, composition is more assorted in the extract of gained, and dose is bigger.(Zhang Jixing such as Zhang Jixing, Li Jian, Deng. the technical study of macroreticular resin absorbing method enrichment Herba Euphorbiae Humifusae total flavones. Chinese crude drug [J] 2002,25 (2): 123～125) adopt the macroporous adsorbent resin method to handle the Herba Euphorbiae Humifusae total flavones, after macroporous resin adsorption extract obtained in content of total flavone be about 16%.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of Herba Euphorbiae Humifusae effective ingredient, in the inventive method, Herba Euphorbiae Humifusae medical material crude extract behind the alkali dissolution acid precipitation, the enrichment of reuse polyamide column, gained effective ingredient impurity is few, composition is comparatively single.
In the Herba Euphorbiae Humifusae owing to contain more flavones ingredient and tannin constituents, flavone is the effective ingredient of Herba Euphorbiae Humifusae, in separation process, because tannin and flavones ingredient structurally have more similar, simple macroporous resin enrichment purification of flavone constituents is brought more tannin class often easily into, and because it all contains more phenolic hydroxyl group, presents certain acidity, when removing other non-acid impurity component with alkali extraction and acid precipitation, tannin is not separated preferably with flavones ingredient.Polyamide be a class to having the stronger resin of chemical compound absorbability of phenolic hydroxyl structure, especially to many ortho-phenolic hydroxyls chemical compound, adsorb very firmly, usually need just can reach the purpose of eluting with alkali.Utilize the absorption characteristics of polyamide, and flavone and tannin become tart character, the present invention adopts the method for alkali extraction and acid precipitation in conjunction with polyamide absorption, purification Herba Euphorbiae Humifusae flavone compound, extract obtained in, flavones ingredient content height, and because in advance through the alkali extraction and acid precipitation step, remove a lot of nonacid composition impurity, handle the loading that the back increases polyamide, the resin of as much can be handled more Herba Euphorbiae Humifusae medical material.
Particularly, preparation technology of the present invention can be:
The Herba Euphorbiae Humifusae medical material is after solvent extracts, gained herbal extract concentrating under reduced pressure, concentrate extracts with alkaline aqueous solution, obtain alkaline water and carry clear liquid, the alkaline water extract filters after transferring pH to 1～4 with acid, must precipitate, precipitate is with after being lower than 10% pure dispersing and dissolving, and last polyamide resin column is handled, and collects the stream part of being rich in flavonoid and promptly gets the Herba Euphorbiae Humifusae activity extract.
In more detail, the preparation method of Herba Euphorbiae Humifusae active component of the present invention is:
The dry medical material of Herba Euphorbiae Humifusae, the ethanol extraction with 50%～80%, ethanol extract merges, be concentrated into the extractum shape, extractum extracts greater than 10 alkali liquor with pH value, filters, and gets the alkaline extraction clear liquid, after the alkali extract is transferred pH to 1～4 with acid, leave standstill, filter, precipitation is washed till the distilled water effluent with distilled water and is neutral, precipitation is disperseed with the ethanol less than 10%, with the polyamide adsorbent resin of having handled well on the dispersion liquid, earlier thin out to the eluent color to be lower than 10% ethanol elution, use 45% to 80% ethanol elution instead, thin out to the eluent color, collect the rear section ethanol elution, merge, concentrate, drying promptly gets the Herba Euphorbiae Humifusae active component extract.
More specifically, the preparation method of active component of the present invention can for:
The dry medical material of Herba Euphorbiae Humifusae, the alcohol reflux with 60%～75% 3 times filters, merge ethanol extract, concentrating under reduced pressure becomes the extractum shape, and extractum extracts 2～3 times with 5%～15% NaOH solution, filter, remove clear liquid, clear liquid is transferred pH to 1～3 with HCl, shakes up, leave standstill, filter, precipitation is washed till water lotion with distilled water and is neutral, and precipitation is again with 5% ethanol dispersing and dissolving, the polyamide adsorbent resin of having handled well on the dispersion liquid, earlier thin out with the pure washing liquid color of 10% ethanol elution to 10%, use 65% ethanol elution instead, thin out to color, the flavonoid reaction is negative, merge 70% ethanol elution, concentrate, be drying to obtain the Herba Euphorbiae Humifusae activity extract.
Among the present invention, medicinal material extract except that being the ethanol, can also be bigger solvent or its aqueous solvents of some polarity such as water, methanol, acetone with solvent, methanol aqueous solution, aqueous acetone solution etc.During extraction, decoct extraction when the present invention is all right, soak extraction, percolation extraction, supersound extraction etc., from medical material as long as the Herba Euphorbiae Humifusae flavones ingredient can be extracted.
Among the present invention, used acid can be inorganic or organic acid such as hydrochloric acid, sulphuric acid, acetic acid, preferred hydrochloric acid; Used alkali can be NaOH, KOH, Na
2CO
3, NaHCO
3, K
2CO
3Or KHCO
3In any.
Several experiments are carried out the result respectively relatively, adopt its content of total flavone of determined by ultraviolet spectrophotometry, the high effective liquid chromatography for measuring quercetin content is to embody advantage of the present invention place.
Experiment one: measure general flavone content, quercetin content among the Herba Euphorbiae Humifusae medical material 1000g.
Experiment two: Herba Euphorbiae Humifusae medical material 1000g, the alcohol reflux with 60% three times filters, merge each time extracting solution, being evaporated to does not have the alcohol flavor, on the AB-8 type macroporous adsorptive resins handled well, earlier thin out to water elution liquid color with water elution, use 60% ethanol elution instead, thin out to 60% ethanol elution color, collect 60% ethanol elution, merge, concentrating under reduced pressure, drying gets extract 61.8g.Measure general flavone content and quercetin content in the extract respectively.
Experiment three: Herba Euphorbiae Humifusae medical material 1000g, the alcohol reflux with 60% three times filters, merge each time extracting solution, be evaporated to into the extractum shape, NaOH aqueous solution dissolving extractum with 5%, filter, get the NaOH clear liquid, the hydrochloric acid with 10% transfers pH to about 3, leave standstill, filter, precipitation is washed till water lotion with distilled water and becomes neutral, the dissolve with ethanol of insoluble matter reuse 10% disperses, with polyamide adsorption resin column on the dispersion liquid, resin is earlier with 10% ethanol elution, and is thin out to the eluent color, use 65% ethanol elution instead, thin out to the eluent color, essentially no flavone reaction, the ethanol elution part of collection 65%, merge, concentrating under reduced pressure, drying gets extract 14.6g.Measure general flavone content and quercetin content in the extract.
The assay method of Quercetin is: remove medical material or extract 1g, the hydrochloric acid with 25%-ethanol liquid refluxes half an hour, after Quercetin glycosides hydrolysis fully, measures its quercetin content again.
The above-mentioned comparing result of respectively testing sees Table 1
Table 1 total flavones, quercetin content result are relatively
From last table result as can be known, just prepare Herba Euphorbiae Humifusae extract with the inventive method, compare with macroporous resin method, no matter general flavone content still be a quercetin content in the extract from extract, all obviously wants height than the macroporous adsorbent resin method.
Specific embodiment
Embodiment 1
Herba Euphorbiae Humifusae medical material 1000g, the alcohol reflux with 50% three times filters, merge each time extracting solution, be evaporated to into the extractum shape, NaOH aqueous solution dissolving extractum with 10%, filter, get the NaOH clear liquid, the hydrochloric acid with 15% transfers pH to about 3.5, leave standstill, filter, precipitation is washed till water lotion with distilled water and becomes neutral, the dissolve with ethanol of insoluble matter reuse 5% disperses, with polyamide adsorption resin column on the dispersion liquid, resin is earlier with 5% ethanol elution, and is thin out to the eluent color, use 45% ethanol elution instead, thin out to the eluent color, essentially no flavone reaction, the ethanol elution part of collection 45%, merge, concentrating under reduced pressure, drying gets extract 12.3g.General flavone content 57.32%, total quercetin content is 11.69%.
Embodiment 2
Herba Euphorbiae Humifusae medical material 1000g, the alcohol reflux with 70% three times filters, merge each time extracting solution, be evaporated to into the extractum shape, KOH aqueous solution dissolving extractum with 5%, filter, get the KOH clear liquid, transfer pH to about 2, leave standstill with 10% hydrochloric acid, filter, precipitation is washed till water lotion with distilled water and becomes neutral, and the dissolve with ethanol of insoluble matter reuse 5% disperses, with polyamide adsorption resin column on the dispersion liquid, resin is earlier with 5% ethanol elution, thin out to the eluent color, use 80% ethanol elution instead, thin out to the eluent color, essentially no flavone reaction, the ethanol elution part of collection 80% merges concentrating under reduced pressure, dry, get extract 17.9g, general flavone content is 46.7%, and total quercetin content is 9.58%.
Embodiment 3
Herba Euphorbiae Humifusae medical material 1000g, the alcohol reflux with 80% 2 times filters, and merges each time extracting solution, is evaporated to into the extractum shape, the Na with 10%
2CO
3Aqueous solution dissolving extractum filters, and gets Na
2CO
3Clear liquid, sulphuric acid with 10% transfers pH to about 3, leave standstill, filter, precipitation is washed till water lotion with distilled water and becomes neutral, the dissolve with ethanol of insoluble matter reuse 15% disperses, with polyamide adsorption resin column on the dispersion liquid, resin is earlier with 15% ethanol elution, and is thin out to the eluent color, use 55% ethanol elution instead, thin out to the eluent color, essentially no flavone reaction, the ethanol elution part of collection 70%, merge, concentrating under reduced pressure, drying gets extract 11.6g, general flavone content is 60.12%, and total quercetin content is 12.34%.
Embodiment 4
Herba Euphorbiae Humifusae medical material 1000g, the alcohol reflux with 60% three times filters, and merges each time extracting solution, is evaporated to into the extractum shape, the K with 5%
2CO
3Aqueous solution dissolving extractum filters, and gets K
2CO
3Clear liquid, hydrochloric acid with 5% transfers pH to about 2, leave standstill, filter, precipitation is washed till water lotion with distilled water and becomes neutral, the dissolve with ethanol of insoluble matter reuse 5% disperses, with polyamide adsorption resin column on the dispersion liquid, resin is earlier with 5% ethanol elution, and is thin out to the eluent color, use 50% ethanol elution instead, thin out to the eluent color, essentially no flavone reaction, the ethanol elution part of collection 50%, merge, concentrating under reduced pressure, drying gets extract 15.8g, general flavone content is 51.7%, and total quercetin content is 9.97%.
Embodiment 5
Herba Euphorbiae Humifusae medical material 1000g, the alcohol reflux with 55% three times filters, and merges each time extracting solution, is evaporated to into the extractum shape, the KHCO with 5%
3Aqueous solution dissolving extractum filters, and gets KHCO
3Clear liquid, hydrochloric acid with 5% transfers pH to about 3, leave standstill, filter, precipitation is washed till water lotion with distilled water and becomes neutral, the dissolve with ethanol of insoluble matter reuse 8% disperses, with polyamide adsorption resin column on the dispersion liquid, resin is earlier with 8% ethanol elution, and is thin out to the eluent color, use 65% ethanol elution instead, thin out to the eluent color, essentially no flavone reaction, the ethanol elution part of collection 65%, merge, concentrating under reduced pressure, drying gets extract 13.7g, general flavone content is 52.4%, and total quercetin content is 10.18%.
Claims (8)
1, a kind of preparation method of Herba Euphorbiae Humifusae effective ingredient, it is characterized in that the Herba Euphorbiae Humifusae medical material is after solvent extracts, gained herbal extract concentrating under reduced pressure, concentrate extracts with alkaline aqueous solution, obtains alkaline water and carries clear liquid, after the alkaline water extract is transferred pH to 1～4 with acid, filter, must precipitate, precipitate is with after being lower than 10% pure dispersing and dissolving, last polyamide resin column is handled, and collects the stream part of being rich in flavonoid and promptly gets the Herba Euphorbiae Humifusae activity extract.
2, preparation method as claimed in claim 1, it is characterized in that the dry medical material of Herba Euphorbiae Humifusae, ethanol extraction with 50%～80%, ethanol extract merges, and is concentrated into the extractum shape, and extractum extracts greater than 10 alkali liquor with pH value, filter, get the alkaline extraction clear liquid, the alkali extract leaves standstill after transferring pH to 1～4 with acid, filter, precipitation is washed till the distilled water effluent with distilled water and is neutral, and precipitation is disperseed with the ethanol less than 10%, with the polyamide adsorbent resin of having handled well on the dispersion liquid, earlier thin out to the eluent color to be lower than 10% ethanol elution, use 45% to 80% ethanol elution instead, thin out to the eluent color, collect the rear section ethanol elution, merge, concentrate, drying promptly gets the Herba Euphorbiae Humifusae active component extract.
3, preparation method as claimed in claim 2, it is characterized in that the dry medical material of Herba Euphorbiae Humifusae, alcohol reflux with 60%～75% 3 times filters, and merges ethanol extract, concentrating under reduced pressure becomes the extractum shape, extractum extracts 2～3 times with 5%～15% NaOH solution, filters, and removes clear liquid, clear liquid is transferred pH to 1～3 with HCl, shake up, leave standstill, filter, precipitation is washed till water lotion with distilled water and is neutral, precipitation is again with 5% ethanol dispersing and dissolving, and the polyamide adsorbent resin of having handled well on the dispersion liquid is thin out with the pure washing liquid color of 10% ethanol elution to 10% earlier, use 65% ethanol elution instead, thin out to color, the flavonoid reaction is negative, and merges 70% ethanol elution, concentrate, be drying to obtain the Herba Euphorbiae Humifusae activity extract.
4, preparation method as claimed in claim 1 or 2 is characterized in that described alkali liquor can be NaOH, KOH, Na
2CO
3, NaHCO
3, K
2CO
3Or KHCO
3In any.
5, preparation method as claimed in claim 1 or 2 is characterized in that described acid can be hydrochloric acid or sulphuric acid.
6,, it is characterized in that the content of flavones ingredient in the described Herba Euphorbiae Humifusae activity extract should be not less than 40% as the described preparation method of arbitrary claim in the claim 1,2 or 3.
7, preparation method as claimed in claim 4 is characterized in that flavones ingredient content is preferably in the Herba Euphorbiae Humifusae activity extract to be not less than 50%.
8, preparation method as claimed in claim 4 is characterized in that described total flavones sign property composition is a Quercetin, and the total amount of Quercetin is 8%～13% in this extract.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810103792XA CN101249132A (en) | 2008-04-11 | 2008-04-11 | Preparation technique of humifuse euphorbia effective ingredient |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810103792XA CN101249132A (en) | 2008-04-11 | 2008-04-11 | Preparation technique of humifuse euphorbia effective ingredient |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101249132A true CN101249132A (en) | 2008-08-27 |
Family
ID=39952843
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA200810103792XA Pending CN101249132A (en) | 2008-04-11 | 2008-04-11 | Preparation technique of humifuse euphorbia effective ingredient |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101249132A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102302538A (en) * | 2011-09-01 | 2012-01-04 | 山东华尔康兽药有限公司 | Humifuse euphorbia herb extract, preparation process and application thereof |
| CN102429951A (en) * | 2011-12-01 | 2012-05-02 | 燕山大学 | Flavone-saponin extract of humifuse euphorbia herb and application thereof |
| CN103655677A (en) * | 2013-12-10 | 2014-03-26 | 大兴安岭嘉迪欧营养原料有限公司 | Novel method for extracting total flavone from humifuse euphorbia herb |
-
2008
- 2008-04-11 CN CNA200810103792XA patent/CN101249132A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102302538A (en) * | 2011-09-01 | 2012-01-04 | 山东华尔康兽药有限公司 | Humifuse euphorbia herb extract, preparation process and application thereof |
| CN102429951A (en) * | 2011-12-01 | 2012-05-02 | 燕山大学 | Flavone-saponin extract of humifuse euphorbia herb and application thereof |
| CN102429951B (en) * | 2011-12-01 | 2013-12-18 | 燕山大学 | Flavone-saponin extract of humifuse euphorbia herb and application thereof |
| CN103655677A (en) * | 2013-12-10 | 2014-03-26 | 大兴安岭嘉迪欧营养原料有限公司 | Novel method for extracting total flavone from humifuse euphorbia herb |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101244129B (en) | Lhasa rhubarb extract, preparation method, and application in preparing preparation for treating cardiovascular and cerebrovascular diseases | |
| CN101985421B (en) | Method for simultaneously preparing chlorogenic acid and luteoloside from honeysuckle flower | |
| CN101336987A (en) | Preparation method of total flavone of Hovenia dulcisThunb | |
| CN101336978A (en) | Extraction method of total flavone of Hovenia dulcisThunb | |
| CN102641326B (en) | Astragalus extract, as well as preparation and application methods thereof | |
| CN102101840A (en) | Method for extracting and separating high-purity 1-Deoxynojirimycin from folium mori | |
| CN104523771A (en) | Ginkgo leaf total flavones and preparing method thereof | |
| CN101856435B (en) | Preparation method and content measurement method of Daphne giraldii Nitsche total coumarin extract | |
| DK2650301T3 (en) | PROCEDURE FOR THE PREPARATION OF ALBIFLORINE AND PAEONIFLORINE | |
| CN105130759A (en) | Extraction method of magnolia officinalis extract | |
| CN101249132A (en) | Preparation technique of humifuse euphorbia effective ingredient | |
| CN113402574B (en) | Method for separating and purifying flavonoids compounds in ethyl acetate phase of polygonum multiflorum by high-speed counter-current chromatography | |
| CN105079564A (en) | Preparation method of fructus forsythiae antidotal tablet | |
| CN102872195B (en) | A kind of preparation method and application thereof of Chinese cassia tree total polyphenols extract | |
| CN100388940C (en) | Quality control method of Chinese medicinal preparation for treating child hyperpyrexia | |
| CN101940642A (en) | Chinese medicinal composition and application thereof | |
| CN101982184A (en) | Preparation method of taraxacum extract | |
| CN103479711B (en) | Application of eucommia ulmoides lignans extracts in preparation of medicine treating renal interstitial fibrosis | |
| CN102429994B (en) | Compound heartleaf houttuynia herb mixture and preparation method thereof | |
| CN102690359B (en) | A kind of method extracting starch and cucurbitacin from Fructus Momordicae tuber | |
| CN106361811B (en) | One kind is promoted blood circulation pharmaceutical composition and preparation method thereof | |
| CN102234299B (en) | Separation method of hyperin | |
| CN104725449A (en) | Paeoniflorin extracting method | |
| CN103123343A (en) | Quality control method for Songling Xuemaikang capsules | |
| CN101780122B (en) | Preparation method of a water-soluble gingko extract |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20080827 |