CN102302554A - Extraction method of schisandra total lignans - Google Patents
Extraction method of schisandra total lignans Download PDFInfo
- Publication number
- CN102302554A CN102302554A CN201110273180A CN201110273180A CN102302554A CN 102302554 A CN102302554 A CN 102302554A CN 201110273180 A CN201110273180 A CN 201110273180A CN 201110273180 A CN201110273180 A CN 201110273180A CN 102302554 A CN102302554 A CN 102302554A
- Authority
- CN
- China
- Prior art keywords
- concentrated solution
- fructus schisandrae
- powder
- schisandrae chinensis
- schisandra
- 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.)
- Granted
Links
Images
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses an extraction method of schisandra total lignans. The method comprises the following steps: (1) crushing a schisandra medicinal material into medium powder for later use; (2) soaking the crushed medicinal material powder with 40-60 percent ethanol for 12 to 36 hours, percolating, and concentrating the percolate at reduced pressure to obtain concentrated solution for later use, wherein the ratio of the volume of the concentrated solution to the weight of the medicinal material is (1-3):1; (3) regulating the concentration of ethanol in the concentrated solution to 80 to 95 percent, and filtering; (4) purifying the filtrate with an alumina column, receiving column passing solution, decoloring with activated carbon for 0.5 to 2 hours at room temperature, and filtering, wherein the dosage of activated carbon is 0.1 to 0.2 percent; and (5) concentrating the filtrate at reduced pressure, drying in vacuum to obtain yellow or brownish yellow solid schisandra total lignans. The extraction method has the advantages of convenience, low energy consumption and the like, and the yield of extracted total lignans is high; and the purification method has the advantages of strong selectivity, complete impurity removal and the like and the purity of total lignans is high.
Description
Technical field
The present invention relates to a kind of method for distilling of Fructus Schisandrae Chinensis total lignanoid, particularly a kind of alcohol percolation method extracts the method for Fructus Schisandrae Chinensis total lignanoid, belongs to the Chinese medicine extraction technical field.
Background technology
(Schisandra chinensis (Turcz.) Ball. is the dry mature fruit of the perennial fallen leaves of Magnoliaceae bejuco to Fructus Schisandrae Chinensis; Its medication is with a long history; Beginning is stated from Shennong's Herbal, is classified as top gradely, has that convergence is astringent or styptic treatment for spontaneous sweating, an effect of supplementing QI for promoting the production of body fluid, kidney calming.Recent studies proves, lignanoid also has multiple effects such as central nerve inhibition, antioxidation, anticancer, blood pressure regulation in the Fructus Schisandrae Chinensis except that having function for protecting liver and reducing enzyme activity, is a kind of genuine northern rare Chinese medicine.The Chinese patent medicine of selling on the market that contains Fructus Schisandrae Chinensis has folk prescription and compound recipe at present, and is various in style, but is crude preparation by using, and active constituent content is low, and dose is bigger, and because the existence of a large amount of inert matters is prone to cause the generation of some untoward reaction.
At present, according to the document record, the extraction process of Fructus Schisandrae Chinensis total lignanoid has CO
2Supercritical extraction technique, ethanol reflux extraction and percolation; Purifying process has silica gel alumina mixture chromatography, macroreticular resin absorbing method.This patent works out a kind of Fructus Schisandrae Chinensis total lignanoid efficiently extracting and purifying new method through contrast test.
The present invention carries out the advanced person's of current trend CO respectively
2Supercritical extraction technique, traditional ethanol refluxing process and percolation extract contrast experiment's research of total lignans in the Fructus Schisandrae Chinensis.Result of study shows: CO
2Supercritical extraction requires equipment cost high, extracts poor selectivity, and the liposoluble constituent that extracts wherein contains a large amount of seed of Fructus Schisandrae Chinensis oil, volatile oil, contains Fructus Schisandrae Chinensis total lignanoid only 12.5%, causes fat-soluble Fructus Schisandrae Chinensis total lignanoid purifying process difficulty to strengthen.The traditional handicraft ethanol reflux extraction needs long-time heating, finds in the experiment, and the long period heating can cause the destruction of total lignans constituents, causes total lignans content to descend.In addition, reflux, extract, consumption quantity of solvent is bigger, and the concentration time of medicinal liquid is long, and energy consumption is high, process cycle is long.The percolation solvent of bibliographical information is a high concentration ethanol, causes Fructus Schisandrae oil and volatile oil to be extracted out, and we adopt high concentration ethanol percolation different from the past; Use the low-concentration ethanol percolation, carry out under the room temperature, both avoided the destruction of hot reflux effective ingredient; Yield is high, practices thrift solvent; Overcome CO again
2Supercritical extraction is to the extracts active ingredients poor selectivity, shortcomings such as equipment cost height; Be not less than at the Fructus Schisandrae Chinensis total lignanoid extraction ratio under the prerequisite of high concentration ethanol extraction ratio; Adopt the suitable low-concentration ethanol percolation that Fructus Schisandrae oil and volatile oil are extracted; Making the total lignans yield up to (with respect to medical material) more than 1%, is 1.25 times of pharmacopeia extraction method.Total rate of transform is up to more than 95%, and purity reaches 70%.Simultaneously, the extraction for active ingredient such as polysaccharide, organic acid in the comprehensive utilization medicinal residues lays the foundation.
Lignanoids belongs to nonpolarity element, and the macroporous resin (nonpolar and low pole) of using current trend carries out purification.Select for use HPD-100 type macroporous resin and alumina column chromatography to carry out contrast experiment's research.Result of study shows: because lignanoids belongs to liposoluble constituent, the upper prop liquid of purification by macroporous resin Fructus Schisandrae Chinensis total lignanoid is suspendible, and stifled post phenomenon very easily takes place, and causes experimental period long; Upper prop absorption is bad, and impurity and total lignans while are had only unsaturatedly just can make it initial gross separation by eluting during the eluting of saturated back, cause the macroporous resin utilization rate low, and purification effect is bad, and the rate of transform is also low; Eluting has been used poisonous, inflammable, explosive organic solvents such as chloroform, petroleum ether, methanol, acetone, and cost is high, poor stability, contaminated environment; And purge process is complicated, and the production cycle is long.Advantages such as the aluminium oxide that we select has low price for the column chromatography material, and it is easy to regenerate, experimentation show that Fructus Schisandrae Chinensis high concentration alcohol liquid is through alumina column, and selectivity is strong, and most of impurity is eliminated, and the total lignans rate of transform reaches more than 95%.Suitability for industrialized is produced.
Summary of the invention
Fructus Schisandrae Chinensis total lignanoid method for distilling yield was low in the past, content is low, energy consumption is high, the production cycle is long in order to overcome, the shortcoming of contaminated environment, and one of the object of the invention is to provide a kind of highly effective extraction method of Fructus Schisandrae Chinensis total lignanoid.The highly effective extraction method of Fructus Schisandrae Chinensis total lignanoid of the present invention comprises the steps:
(1) schisandra chinensis medicinal material is ground into middle powder, subsequent use;
(2) to use mass fraction be 40%～60% soak with ethanol 12-36h to the medicinal powder after will pulverizing, percolation, and the percolate concentrating under reduced pressure obtains concentrated solution, and described concentrated solution volume (ml) and used medical material weight (g) are than being 1～3: 1, and concentrated solution is subsequent use;
(3) concentration of alcohol in the concentrated solution is heightened to mass fraction be 80%～95%, filter;
(4) filtrating was collected post liquid through the alumina column purification, crossed post liquid and carried out activated carbon decolorizing, and decolorization condition is the 0.5～2h that decolours under the room temperature, filters;
(5) filtrate decompression concentrates, vacuum drying, drying condition be pressure-0.06Mpa～-0.1Mpa, 40 ℃～80 ℃ of temperature promptly obtain yellow or the solid-state Fructus Schisandrae Chinensis total lignanoid of pale brown color.
In specific embodiment of the present invention, preferred, the middle powder described in the step (1) is for the order number is the above powder of 65 orders, and what wherein contained can be no more than 60% of said middle grain weight amount through the powder of 80 mesh sieves.
In specific embodiment of the present invention, preferred, the aluminium oxide described in the step (4) is before use through 110 ℃ of activation 6 hours.
In specific embodiment of the present invention, preferred, aluminium oxide and medicinal powder weight ratio are 8～12: 1 described in the step (4).
In specific embodiment of the present invention, preferred, in the activated carbon decolorizing described in the step (4), every 100ml crosses that amount of activated is 0.1-0.2g in the post liquid.
The flow chart of the method for distilling of Fructus Schisandrae Chinensis total lignanoid of the present invention as shown in Figure 1.
Another object of the present invention provides the Fructus Schisandrae Chinensis total lignanoid that is prepared by above-described method.
The present invention adopts low concentration (immersion, percolation under 40～60%w/w) the ethanol room temperatures according to oil-soluble composition Fructus Schisandrae Chinensis vegetable oil, volatile oil deliquescent difference in different concentration ethanol of Fructus Schisandrae Chinensis total lignanoid and coexistence.Do not contain Fructus Schisandrae oil and volatile oil in the percolate, contained Fructus Schisandrae Chinensis total lignanoid is 1～1.25% of a medical material, is 1.25 times of pharmacopeia methanol ultrasonic extraction method.Overcome CO
2Supercritical extraction extracts Fructus Schisandrae oil and volatile oil with Fructus Schisandrae Chinensis total lignanoid together, causes the shortcoming that Fructus Schisandrae Chinensis total lignanoid purity is low, separation and purification is difficult.The present invention is not less than under the prerequisite of high concentration ethanol extraction at low-concentration ethanol extraction Fructus Schisandrae Chinensis total lignanoid according to the fat-soluble characteristics of Fructus Schisandrae Chinensis total lignanoid, though Fructus Schisandrae oil and volatile oil are not suggested, water-soluble components is corresponding increase in extracting solution.According to this situation, adopt the percolate concentrating under reduced pressure targetedly, concentrated solution is heightened concentration of alcohol, causes most of water-soluble components and is gone out by deposition; Another part is not coexisted with Fructus Schisandrae Chinensis total lignanoid in high concentration ethanol solution by sedimentary water-soluble components; Selected alumina column chromatography targetedly; Utilize aluminium oxide optionally adsorbed water solubility impurity and characteristics of not adsorbing Fructus Schisandrae Chinensis total lignanoid in high concentration ethanol solution; Successfully with the Fructus Schisandrae Chinensis total lignanoid purification; Aluminium oxide with this understanding; Adsorb Fructus Schisandrae Chinensis total lignanoid hardly, the rate of transform is more than 95%, and the Fructus Schisandrae Chinensis total lignanoid purity that obtains reaches more than 70%.It is easy that this method for distilling has extraction process, and the total lignans yield of extraction high (1～1.25%), the rate of transform high (95%), purity high (70%) are practiced thrift cost, and safety is good, environmental protection, production efficiency advantages of higher.The upper prop liquid that has overcome the purification by macroporous resin Fructus Schisandrae Chinensis total lignanoid is suspendible, and stifled post phenomenon very easily takes place, and causes experimental period long; Upper prop absorption is bad, and impurity and total lignans have only unsaturatedly just can make it initial gross separation simultaneously by eluting during the eluting of saturated back, cause the macroporous resin utilization rate low, and purification effect is bad, and the rate of transform is low, the shortcoming of process cycle length.Overcome alumina adsorption Fructus Schisandrae Chinensis total lignanoid crude extract again with silica gel mixing upper prop eluting; Owing to be eluting again after the absorption; Eluting is incomplete; The rate of transform is low; Eluting has been used poisonous, inflammable, explosive organic solvents such as chloroform, petroleum ether, methanol, acetone; Cost is high, long, poor stability of production cycle, the shortcoming of contaminated environment.
Description of drawings
The flow chart of the method for distilling of Fig. 1 high-purity schisandra total lignan of the present invention.
The specific embodiment
Further describe the present invention below in conjunction with specific embodiment, advantage of the present invention and characteristics will be more clear along with description.But these embodiment only are exemplary, scope of the present invention are not constituted any restriction.It will be understood by those skilled in the art that and down can make amendment with form or replace without departing from the spirit and scope of the present invention, but these modifications and replacing all fall in protection scope of the present invention the details of technical scheme of the present invention.
Embodiment 1
A kind of method for distilling of Fructus Schisandrae Chinensis total lignanoid comprises the steps:
(1) schisandra chinensis medicinal material is ground into middle powder (powder is more than 65 orders, can be no more than 60% through the powder of 80 mesh sieves but be mixed with), subsequent use; (2) to use mass fraction be percolation behind the 50% soak with ethanol 36h to the medicinal powder after will pulverizing, and collects the percolate of 10 times of amounts of medical material (ml/g), and the percolate concentrating under reduced pressure obtains concentrated solution, and concentrated solution volume (ml) and used medical material weight (g) are than being 3: 1, and is subsequent use; (3) concentrated solution is heightened concentration of alcohol to containing alcohol amount 80% (w/w), leached insoluble matter, filtrate for later use; (4) 12 times of weight of medical material (w/w) alumina column (aluminium oxide is with 110 ℃ on preceding warp activation 6h) purification of filtrating through 0.2% (w/v, the active carbon that is added in the 100ml filtrating is 0.2g) activated carbon decolorizing 2h, filters again, and is subsequent use; (5) filtrate decompression concentrates ,-0.06Mpa, under 80 ℃ of conditions of temperature, vacuum drying obtains yellow or the solid-state Fructus Schisandrae Chinensis total lignanoid of pale brown color.
Yield 1%, total rate of transform 95%, purity 70%.
Embodiment 2
A kind of method for distilling of Fructus Schisandrae Chinensis total lignanoid comprises the steps:
(1) schisandra chinensis medicinal material is ground into middle powder (powder is more than 65 orders, can be no more than 60% through the powder of 80 mesh sieves but be mixed with), subsequent use; (2) to use mass fraction be percolation behind the 55% soak with ethanol 24h to the medicinal powder after will pulverizing, and collects the percolate of 10 times of amounts of medical material (ml/g), and the percolate concentrating under reduced pressure obtains concentrated solution, and concentrated solution volume (ml) and used medical material weight (g) are than being 2: 1, and is subsequent use; (3) concentrated solution is heightened concentration of alcohol to containing alcohol amount 90% (w/w), leached insoluble matter, filtrate for later use; (4) 10 times of weight of medical material (w/w) alumina column (aluminium oxide is with 110 ℃ on preceding warp activation 6h) purification of filtrating through 0.2% (w/v, the active carbon that is added in the 100ml filtrating is 0.2g) activated carbon decolorizing 1h, filters again, and is subsequent use; (5) filtrate decompression concentrates ,-0.08Mpa, under 60 ℃ of conditions of temperature, vacuum drying obtains yellow or the solid-state Fructus Schisandrae Chinensis total lignanoid of pale brown color.
Yield 1.2%, total rate of transform 95.2%, purity 70.3%.
Embodiment 3
A kind of method for distilling of Fructus Schisandrae Chinensis total lignanoid comprises the steps:
(1) schisandra chinensis medicinal material is ground into middle powder (powder is more than 65 orders, can be no more than 60% through the powder of 80 mesh sieves but be mixed with), subsequent use; (2) to use mass fraction be percolation behind the 60% soak with ethanol 12h to the medicinal powder after will pulverizing, and collects the percolate of 10 times of amounts of medical material (ml/g), and the percolate concentrating under reduced pressure obtains concentrated solution, and concentrated solution volume (ml) and used medical material weight (g) are than being 1: 1, and is subsequent use; (3) concentrated solution is heightened concentration of alcohol to containing alcohol amount 95% (w/w), leached insoluble matter, filtrate for later use; (4) filtrated alumina column (aluminium oxide is with 110 ℃ on the preceding warp activation 6h) purification of 8 times of weight of medical material (w/w), 0.1% (w/v, the active carbon that is added in the 100ml filtrating is 0.1g) activated carbon decolorizing 0.5h, subsequent use; (5) filtrate decompression concentrates ,-0.1Mpa, under 40 ℃ of conditions of temperature, vacuum drying obtains yellow or the solid-state Fructus Schisandrae Chinensis total lignanoid of pale brown color.
Yield 1.25%, total rate of transform 95.4%, purity 70.5%.
Claims (6)
1. the method for distilling of a Fructus Schisandrae Chinensis total lignanoid is characterized in that comprising the steps:
(1) schisandra chinensis medicinal material is ground into middle powder, subsequent use;
(2) to use mass fraction be 40%～60% soak with ethanol 12-36h to the medicinal powder after will pulverizing, percolation, and the percolate concentrating under reduced pressure obtains concentrated solution, and described concentrated solution volume (ml) and used medical material weight (g) are than being 1～3: 1, and concentrated solution is subsequent use;
(3) concentration of alcohol in the concentrated solution is heightened to mass fraction be 80%～95%, filter;
(4) filtrating was collected post liquid through the alumina column purification, crossed post liquid and carried out activated carbon decolorizing, and decolorization condition is the 0.5～2h that decolours under the room temperature, filters;
(5) filtrate decompression concentrates, vacuum drying, drying condition be pressure-0.06Mpa～-0.1Mpa, 40 ℃～80 ℃ of temperature promptly obtain yellow or the solid-state Fructus Schisandrae Chinensis total lignanoid of pale brown color.
2. according to the described method of claim 1, it is characterized in that: the middle powder described in the step (1) is for the order number is the above powder of 65 orders, and what wherein contained can be no more than 60% of said middle grain weight amount through the powder of 80 mesh sieves.
3. according to the described method of claim 1, it is characterized in that: the aluminium oxide described in the step (4) is before use through 110 ℃ of activation 6 hours.
4. according to claim 1 or 3 described methods, it is characterized in that: aluminium oxide described in the step (4) and medicinal powder weight ratio are 8～12: 1.
5. according to the described method of claim 1, it is characterized in that: in the activated carbon decolorizing described in the step (4), every 100ml crosses that amount of activated is 0.1-0.2g in the post liquid.
6. the Fructus Schisandrae Chinensis total lignanoid for preparing according to each described method of claim 1-5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110273180 CN102302554B (en) | 2011-09-15 | 2011-09-15 | Extraction method of schisandra total lignans |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110273180 CN102302554B (en) | 2011-09-15 | 2011-09-15 | Extraction method of schisandra total lignans |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102302554A true CN102302554A (en) | 2012-01-04 |
| CN102302554B CN102302554B (en) | 2013-08-07 |
Family
ID=45376537
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110273180 Expired - Fee Related CN102302554B (en) | 2011-09-15 | 2011-09-15 | Extraction method of schisandra total lignans |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102302554B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112057500A (en) * | 2020-10-16 | 2020-12-11 | 陕西嘉禾药业有限公司 | Method for extracting polysaccharide, volatile oil, flavone and lignan from schisandra chinensis |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101057887A (en) * | 2007-05-16 | 2007-10-24 | 徐海波 | Northern schisandra stems or stems skin extraction, its preparation method and application |
| CN101214278A (en) * | 2007-12-26 | 2008-07-09 | 沈阳药科大学 | New raw material for extracting fructus schizandrae total lignans and preparation technique and use |
| CN101973856A (en) * | 2010-10-19 | 2011-02-16 | 南京泽朗医药科技有限公司 | Process for extracting schizandrin A from schizandra |
-
2011
- 2011-09-15 CN CN 201110273180 patent/CN102302554B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101057887A (en) * | 2007-05-16 | 2007-10-24 | 徐海波 | Northern schisandra stems or stems skin extraction, its preparation method and application |
| CN101214278A (en) * | 2007-12-26 | 2008-07-09 | 沈阳药科大学 | New raw material for extracting fructus schizandrae total lignans and preparation technique and use |
| CN101973856A (en) * | 2010-10-19 | 2011-02-16 | 南京泽朗医药科技有限公司 | Process for extracting schizandrin A from schizandra |
Non-Patent Citations (2)
| Title |
|---|
| 于俊林等: "北五味子根、茎、叶与果实木脂素成分比较研究", 《人参研究》 * |
| 芦金清等: "五味子提取工艺的研究", 《中成药》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112057500A (en) * | 2020-10-16 | 2020-12-11 | 陕西嘉禾药业有限公司 | Method for extracting polysaccharide, volatile oil, flavone and lignan from schisandra chinensis |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102302554B (en) | 2013-08-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101744886B (en) | Method for extracting high-purity schisandra total lignan | |
| CN1066055C (en) | Production method for extracting flavonoid compound extract or powder from bamboo leaf | |
| CN106588616B (en) | A kind of preparation method of curcumin | |
| CN102976909B (en) | Method for extracting and purifying 6-gingerol from ginger | |
| CN101274953B (en) | Method for extracting corosolic acid from plant | |
| CN112870236B (en) | Flavone effective part of abelmoschus manihot and preparation method and application thereof | |
| CN101721452A (en) | New process for improving utilization ratio of lithospermum | |
| CN101074188B (en) | Method for enriching and purifying veralkcohol from peanut root by macporous adsorptive resin | |
| CN105503786B (en) | Split Lignanoids compounds-smartweed diffractive ring lignan glucoside E and preparation method thereof | |
| CN103480178A (en) | Method for extracting active ingredients from coreopsis tinctoria by subcritical water | |
| CN101747195B (en) | Separation and purifying method for DCQA (dicaffeoylquinic acid) component in jerusalem artichoke | |
| CN103494858A (en) | Method for enriching total flavonoids in taraxacum mongolicum with macroporous resins | |
| CN104000935B (en) | A kind of method that anti-oxidant phenolic acid is extracted in the slag from jacket | |
| CN102302554B (en) | Extraction method of schisandra total lignans | |
| CN102688284A (en) | Preparation method of lavender total flavone | |
| CN105294793B (en) | The separation method of aurantiin in aizoon stonecrop | |
| CN102533446B (en) | Method for removing furocoumarins from citrus essential oil | |
| CN102070569B (en) | Method for enriching and purifying 3,4-divanillyltetrahydrofuran in nettle | |
| CN104189073B (en) | The preparation method of salvianolic acid | |
| CN101899083B (en) | Preparation method of cyclocarya paliurus acid A | |
| CN102920783B (en) | Process for preparing effective components of schisandrachinensis | |
| CN102643318B (en) | Method for extracting refined cordycepin from Cordyceps militaris fruit body | |
| CN102199156A (en) | Preparation of gelsemine from gelsemium extract by using chromatography | |
| CN112851621A (en) | Total iridoid extract of caulis et folium piperis, extraction and purification method and application thereof | |
| CN101926811A (en) | Triterpenoid saponin total extract of Chinese starjasmine stem and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130807 Termination date: 20140915 |
|
| EXPY | Termination of patent right or utility model |