CN102670680A - Method for extracting total saponins from bark of acanthopanax brachypus harms - Google Patents
Method for extracting total saponins from bark of acanthopanax brachypus harms Download PDFInfo
- Publication number
- CN102670680A CN102670680A CN 201210182016 CN201210182016A CN102670680A CN 102670680 A CN102670680 A CN 102670680A CN 201210182016 CN201210182016 CN 201210182016 CN 201210182016 A CN201210182016 A CN 201210182016A CN 102670680 A CN102670680 A CN 102670680A
- Authority
- CN
- China
- Prior art keywords
- extraction
- total saponins
- solvent
- acanthopanax brachypus
- acanthopanax
- 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
Images
Abstract
The invention relates to a method for extracting total saponins from bark of acanthopanax brachypus harms, and belongs to the field of extraction of active ingredients of natural products. The process flow is that the bark of acanthopanax brachypus harms is taken as raw materials, the mixed solvent of [Bmin]Br and water is taken as extraction solvent, continuous flowing extraction is performed through ultrasonic-microwave collaborative solvent, extraction process is detected through an IR detector, and filter liquor is deposited and centrifuged to obtain clear extracting solution; and the extracting solution is degreased through diethyl ether and is subjected to macroporous absorption resin column chromatography, so that 70% of ethanolic elution is collected, discolored through activated carbon, and impurities are removed through aluminum oxide so as to obtain total saponins. After analysis, the extraction rate achieves more than 8.56%, the content of the total saponins achieves more than 92.53%, and is higher than that of the total saponins obtained by other methods. The method has the advantages of normal pressure extraction, simple process, quickness and simplicity in operation, energy conservation and environmental friendliness and high selectivity, and can perform on-line detection to the extraction process; the saponin is not easy to denature, and does not need to be filtered and separated after extraction; and the extraction rate and purity of the total saponins are high, and the industrialized production can be facilitated.
Description
Technical field
The present invention relates to active ingredient of natural product and extract the field, relate in particular to a kind of method of from the Acanthopanax brachypus peel of stem, extracting total saponins.
Background technology
At present; Mainly be to extract solvent both at home and abroad with the organic solvent; Adopt technology such as solvent soaking, Suo Shi extraction, reflux, ultrasonic-assisted extraction and microwave-assisted extraction to extract the effective ingredient in the natural product; But all there is extraction time length to some extent in these technology, solvent load is many, toxicity is big, extraction ratio is low, the effective ingredient destructible, is difficult to realize deficiencies such as online detection, have greatly restricted the application of these technology in active ingredient of natural product extracts.Ionic liquid is a kind of environmental type solvent; Very high polarizability is arranged; Microwave had strong absorption and hot transfer capability; Have also that solvability is strong, steam forces down, unique physical and chemical properties such as volatility is little, liquid wide ranges, can be used as the solvent that microwave-assisted extracts effective ingredient in the natural product.In addition, the material that the IR spectroscopic data can embody in the sample is formed and structural information, and IR is spectrographic obtains easy and simple to handle and cost is low, need not the complicated sample pre-treatment, is suitable for online detection.
Acanthopanax plant mostly has higher medical value.Clinical and pharmacological research shows that the saponin that is rich in the acanthopanax plant has many-sided pharmacological actions such as antiinflammatory, antitumor, anti-stress, antiviral, cholesterol reducing, blood sugar lowering and immunomodulating.Saponin is an active substance main in the acanthopanax plant, has become the important indicator of weighing the Acanthopanax quality of medicinal material.Acanthopanax brachypus is that China just was exploited in recent years, distinctive medicinal plants among the people; Effect with replenishing QI to invigorate the spleen, tranquilizing by nourishing the heart, resolving depression and blood, the extract of its rhizome have effects such as treatment neurasthenia, male sexual disorder, climacteric syndrome, secondary hypertension, hypotension, leukopenia, cancer-resisting.The inventor is carrying out finding in the systematic study to the chemical constituent of Acanthopanax brachypus, contains abundant saponin component in its peel of stem, through experiment repeatedly, has explored a kind of method of extracting total saponins in the Acanthopanax brachypus peel of stem.
Summary of the invention
In order to overcome the deficiency in the extracts active ingredients technology in the above-mentioned natural product of mentioning, task of the present invention is: design a kind of total saponins that fast and effeciently extracts in the Acanthopanax brachypus peel of stem, can realize the method for the online Detection and Extraction process of IR simultaneously again.
The present invention solves the technical scheme that task adopts:
1, select solvability to Acanthopanax brachypus saponin mixed solvent strong, that ultrasound wave and microwave are had strong absorption and the ionic liquid of hot transfer capability [Bmim] Br (bromination 1-butyl-3-Methylimidazole .) and water as the extraction solvent; The recycle solvent reduces extraction cost, reduces environmental pollution.
2, extracting solvent is continuous-flow, and the solvent that contacts with sample remains fresh, to improve extraction ratio, the online Detection and Extraction process of while IR.
3, utilize hyperacoustic cavitation, machinery and the high energy of cell wall breaking effect and microwave to act on the ultrasonic-microwave cooperating extractive technique of one, to improve extraction ratio, to reduce destruction, the realization suitability for industrialized production of effective ingredient.
4, adopt macroporous adsorptive resins refining, activated carbon decolorizing, the neutral alumina post is removed impurity such as tannin.
The present invention compared with prior art has the following advantages:
1, the mixed solvent with ionic liquid [Bmim] Br and water serves as to extract solvent, and extraction ratio of effective constituents is high, extraction cost is low, environmental pollution is little.
2, extracting solvent is continuous-flow, and the solvent that contacts with sample in the leaching process is fresh all the time, and the dissolution rate of effective ingredient is high; Extract filtrating and in time constantly flows out extraction tube, avoid effective ingredient to cause decomposition because of heated time is long, and extract filtrating and need not to filter, can realize the online Detection and Extraction process of IR.
3, adopt ultrasonic-microwave cooperating extractive technique, extraction time is short, operating procedure is simple, saponin not changeableness, be easy to suitability for industrialized production.
4, the extraction ratio with the Acanthopanax brachypus total saponins serves as to investigate index, extraction conditions is optimized, and compares (referring to table 1) with traditional extraction method.Result of study shows that (the extraction solvent strength is 1.5mol/L, solid-to-liquid ratio 1: 30g/mL in the optimum extraction process condition; Solvent flow rate is 3mL/min, and the extraction tube internal diameter is 50mm, and extraction tube length is 150mm; Microwave power is 600W, and ultrasonic power is 450W, and be 4s/6s ultrasonic off time) under; The extraction ratio of total saponins is 8.56%, apparently higher than other method for distilling.Show that the present invention is a kind of method for distilling of ideal Acanthopanax brachypus total saponins.
Table 1: the extraction ratio of Different Extraction Method relatively
| Method | Solvent | Extraction ratio (%) |
| Ultrasonic-microwave cooperating flow of solvent extraction method | [Bmim]Br/H 2O(1.5mol/L) | 8.56 |
| The microwave-assisted extraction method | [Bmim]Br/H 2O(1.5mol/L) | 7.13 |
| The solvent soaking method | C 2H 5OH/H 2O(95％) | 4.59 |
| Soxhlet extraction | C 2H 5OH/H 2O(95％) | 6.23 |
| Heating reflux method | C 2H 5OH/H 2O(95％) | 5.47 |
| The ultrasonic-assisted extraction method | [Bmim]Br/H 2O(1.5mol/L) | 6.87 |
Description of drawings
Fig. 1 is the apparatus structure sketch map that from the Acanthopanax brachypus peel of stem, extracts total saponins that the present invention relates to.
Fig. 2 is the extraction and the process for refining flow chart of total saponins in the Acanthopanax brachypus peel of stem that the present invention relates to.
Description of reference numerals
The specific embodiment
The extraction of saponin: in Fig. 1; Sample (11) is processed in exsiccant Acanthopanax brachypus peel of stem pulverizing; The sample that the takes by weighing certain mass internal diameter of packing into is that 50mm, length are in the extraction tube (6) of 150mm; An amount of glass cotton (7) of pad is filled out in the sample top and the bottom, with extraction tube microwave oven (1) intracavity of packing into, will be connected the middle that ultrasound probe (5) on the supersonic generator (2) is inserted into sample in the extraction tube through lead (8) simultaneously.By solid-to-liquid ratio is 1: the amount of 30g/mL is prepared the 1.5mol/L of certain volume [Bmim] Br/H
2The extraction solvent (12) of O; And will extract solvent through peristaltic pump (4) and tube for transfusion (10) and be pumped in the extraction tube, open microwave oven and supersonic generator simultaneously, the adjusting solvent flow rate is 3mL/min; Microwave power is 600W; Ultrasonic power is 450W, and be 4s/6s ultrasonic off time, collects and extracts filtrating (13).In leaching process, can open piston (9), through the online Detection and Extraction process of infrared spectrometric analyzer (3).Extract filtrating through precipitate, centrifugal after, obtain clarifying extracting solution.
Extraction ratio with the Acanthopanax brachypus total saponins serves as to investigate index, and extraction conditions is optimized, and obtain the optimum extraction process condition and be: the extraction solvent strength is 1.5mol/L; Solid-to-liquid ratio 1: 30g/mL, solvent flow rate is 3mL/min, the extraction tube internal diameter is 50mm; Extraction tube length is 150mm, and microwave power is 600W, and ultrasonic power is 450W; Be 4s/6s ultrasonic off time, and the extraction ratio of total saponins is 8.56%.
Making with extra care of saponin: extracting solution concentrates behind ether defatting, crosses the D-101 macroporous adsorptive resins, and it is closely colourless that resin is eluted to eluent with deionized water earlier; To remove desaccharide and other water-solubility impurities, the ethanol elution of reuse 70% does not flow down to having saponin constituent basically, and (Butter of antimony .-chloroform saturated solution is a developer in the TLC detection; Reaction is negative) the eluting terminal point, merge alcohol eluen, add the active carbon that is equivalent to quality of medicinal material 1% again; Reflux decolouring 10min, filtered while hot is filtrating is removed impurity such as tannin through the neutral alumina post after; Concentrating under reduced pressure, vacuum drying, pulverizing, grind, sieve, the Acanthopanax brachypus total saponins, extraction ratio is 8.56%.Through the HPLC content analysis, total saponin content is 92.53%.
The present invention has that normal pressure extracts, extracts that flow process is simple, operation is quick and convenient, energy-conserving and environment-protective, selectivity are high, can online Detection and Extraction process, saponin not changeableness, high without isolated by filtration, extraction ratio and purity after extracting, be easy to advantage such as suitability for industrialized production.
Claims (4)
1. the method for distilling of an Acanthopanax brachypus total saponins; It is characterized in that: the Acanthopanax brachypus peel of stem is pulverized, carried out ultrasonic-microwave cooperating extraction with [Bmim] Br of continuous-flow and the mixed solvent of water, with the online Detection and Extraction process of IR; Filtrating obtains clarifying extracting solution through deposition, centrifugal.Extracting solution is behind ether defatting, and it is refining to cross macroporous adsorptive resins, collects 70% ethanol elution, after activated carbon decolorizing and neutral alumina are removed impurity, obtains the Acanthopanax brachypus total saponins again.
2. the method for distilling of a kind of Acanthopanax brachypus total saponins according to claim 1 is characterized in that: the mixed solvent with ionic liquid [Bmim] Br (bromination 1-butyl-3-Methylimidazole .) and water serves as to extract solvent.
3. the method for distilling of a kind of Acanthopanax brachypus total saponins according to claim 1; It is characterized in that: in the leaching process, extracting solvent is continuous-flow, and the solvent that contacts with sample is fresh all the time; Extracting solution in time constantly flows out the extraction system, and the extraction process can be used the online detection of IR.
4. the method for distilling of a kind of Acanthopanax brachypus total saponins according to claim 1 is characterized in that: adopt ultrasonic-microwave cooperating extractive technique.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210182016 CN102670680A (en) | 2012-05-26 | 2012-05-26 | Method for extracting total saponins from bark of acanthopanax brachypus harms |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210182016 CN102670680A (en) | 2012-05-26 | 2012-05-26 | Method for extracting total saponins from bark of acanthopanax brachypus harms |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102670680A true CN102670680A (en) | 2012-09-19 |
Family
ID=46803666
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201210182016 Pending CN102670680A (en) | 2012-05-26 | 2012-05-26 | Method for extracting total saponins from bark of acanthopanax brachypus harms |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102670680A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104435030A (en) * | 2014-11-04 | 2015-03-25 | 吉林省标达科技有限责任公司 | Method for extracting total eleutheroside |
| CN104650175A (en) * | 2014-06-12 | 2015-05-27 | 唐泽光 | Purification method of saponin |
| CN106420855A (en) * | 2016-09-28 | 2017-02-22 | 内蒙古宏魁生物药业有限公司 | Method for leaching saponin and polysaccharide |
| CN106480156A (en) * | 2016-12-04 | 2017-03-08 | 西北大学 | A kind of method of enzyme catalysiss glycol group ginsenoside's large-scale production rare ginsenoside |
| CN106480157A (en) * | 2016-12-04 | 2017-03-08 | 西北大学 | A kind of method of enzyme catalysiss triol group ginsenoside's large-scale production rare ginsenoside |
-
2012
- 2012-05-26 CN CN 201210182016 patent/CN102670680A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104650175A (en) * | 2014-06-12 | 2015-05-27 | 唐泽光 | Purification method of saponin |
| CN104435030A (en) * | 2014-11-04 | 2015-03-25 | 吉林省标达科技有限责任公司 | Method for extracting total eleutheroside |
| CN106420855A (en) * | 2016-09-28 | 2017-02-22 | 内蒙古宏魁生物药业有限公司 | Method for leaching saponin and polysaccharide |
| CN106420855B (en) * | 2016-09-28 | 2020-10-09 | 内蒙古宏魁生物药业有限公司 | Method for leaching saponin and polysaccharide |
| CN106480156A (en) * | 2016-12-04 | 2017-03-08 | 西北大学 | A kind of method of enzyme catalysiss glycol group ginsenoside's large-scale production rare ginsenoside |
| CN106480157A (en) * | 2016-12-04 | 2017-03-08 | 西北大学 | A kind of method of enzyme catalysiss triol group ginsenoside's large-scale production rare ginsenoside |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101797344B (en) | Method for preparing refined total flavonoids in herba lophatheri | |
| CN102276679B (en) | Method for extracting high-purity tea saponin from oil-tea-cake by decompression boiling | |
| CN105037448B (en) | A kind of method that rapid, high volume extracts the separation oligomeric sugar monomer of coix seed | |
| CN102670680A (en) | Method for extracting total saponins from bark of acanthopanax brachypus harms | |
| CN102351819A (en) | Extraction, purification and preparation method of high-purity salvianolic acid B | |
| CN104306428B (en) | A method of the extraction purification gypenoside from gynostemma pentaphylla | |
| CN100439319C (en) | Method for preparing salviol acid A | |
| CN102219814A (en) | Method for extracting aucubin from eucommia ulmoides oliver seed draff | |
| CN105213441A (en) | A kind of technique simultaneously preparing glycosides and Folium hydrangeae strigosae total polyphenols | |
| CN101559090A (en) | Extracting method of steroid saponins of yerbadetajo | |
| CN102617693A (en) | Method and device utilizing subcritical water extraction technology to extract and prepare ursolic acid from loquat leaves | |
| CN104829656B (en) | A kind of method that gentiamarin chemical reference substance is prepared from gentiana straminea | |
| CN108840845A (en) | The method of Xanthatin is extracted from Siberian cocklebur | |
| CN102898347A (en) | Method for extracting caragana microphylla from hypaphorine | |
| CN103664610B (en) | Method for extracting chlorogenic acid from sweet potato leaves | |
| CN108101923B (en) | Separation and purification method of glabridin monomer | |
| CN108042618B (en) | Method for extracting total paeoniflorin by using subcritical water | |
| CN110141605A (en) | A kind of preparation method of snowpoppy total alkaloid nanoparticle | |
| CN103965276B (en) | The method of fast separating and purifying monomeric compound from Lindley Eupatorium Herb | |
| CN102391344A (en) | Method for preparing picfeltarraenin IA from picria feltarrae lour leaves | |
| CN102260152A (en) | Preparation method and medicinal application of shogaol extract | |
| CN104447642B (en) | The preparation of industrialization chromatographic separation and purification method of andrographolide | |
| CN107074798B (en) | Method for extracting phytoxin from rhodiola rosea | |
| CN104059111A (en) | Method for extracting manninotriose monomer from rehmannia by virtue of activated carbon gradient elution | |
| CN110066306A (en) | A kind of Isorhamnetin-3-O-neohespeidoside preparative liquid chromatography separation method |
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: 20120919 |