CN105646464A - Method for extracting high-purity mangiferin from bombax ceiba leaves - Google Patents
Method for extracting high-purity mangiferin from bombax ceiba leaves Download PDFInfo
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- CN105646464A CN105646464A CN201610099728.3A CN201610099728A CN105646464A CN 105646464 A CN105646464 A CN 105646464A CN 201610099728 A CN201610099728 A CN 201610099728A CN 105646464 A CN105646464 A CN 105646464A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D407/00—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00
- C07D407/02—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings
- C07D407/04—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings directly linked by a ring-member-to-ring-member bond
Abstract
The invention relates to a method for extracting high-purity mangiferin from bombax ceiba leaves. The extracting method mainly comprise the steps that the bombax ceiba leaves are taken as the raw material, dried and ground, a product is extracted with an alcoholic solution, alcohol is recovered, and crude mangiferin is obtained; the crude mangiferin is processed with AB-8 macroporous resin for further enrichment and purification; finally, the high-purity mangiferin is obtained through HSCCC (high-speed countercurrent chromatography) separation and purification. The method is simple and reasonable, and the finally obtained product is high in purity and can be widely applied to medicine and hygiene industries.
Description
Technical field
The present invention relates to a kind of method preparing high-purity Fructus Mangifera Indicae, main technique includes alcohol extraction, and macroporous resin decolouring separates with HSCCC.
Background technology
Kapok (BombaxmalabaricumDC) is also known as hero tree, Mo Lian, red jasmine, silk cotton tree, silk cotton, Flos Bombacis Malabarici, speckle Mang Shu etc., for Bombacaceae Gossampinus plant, for deciduous tree, Chang Xianhua posterior lobe, completely set when opening, very grand, it is the common plant of southern china. Kapok is many is used as medicine with flower, bark and root, tool expelling wind and removing dampness, the effect such as promoting blood circulation and detumescence, removing obstruction for relieving pain, it it is one of Nationality in Hainan Province common medicine, among the people mainly take its root, bark, flower or leaf and be decocted in water for oral dose, be used for controlling dysentery, damp-heat diarrhea, woman month endogenous wind, pulmonary carcinoma, intestinal cancer, stomachache, hematochezia and arthromyodynia etc. after an action of the bowels.
Common bombax leaf is the leaf of plant kapok. In recent years, kapok because of its antiinflammatory, antitumor, protect the liver etc. in there is good activity and receive significant attention, but the correlational study of common bombax leaf is less, only in its chemical composition, pharmacological action aspect has a small amount of report. Containing a large amount of chimonins in bibliographical information common bombax leaf, its content is up to 7%. But have not yet to see the relevant report of chimonin extraction process in common bombax leaf.
Chimonin (mangiferin), also known as mangiferin, mangiferin, is a kind of tetrahydroxy pyrrone carbon glycoside, belongs to double; two benzene pyrrones compound. Central nervous system, respiratory system, cardiovascular system all there are is certain effect, acts in addition with antiviral, radioprotective, antitumor, anti-diabetic and hepatic cholagogic etc. Just because of its such purposes widely, the report about chimonin is a lot, and the patent extracting high-purity Fructus Mangifera Indicae is also more, but the report extracting high purity mangiferin from common bombax leaf there is not yet.
Macroporous adsorbent resin is that fast development is got up on the basis of ion exchange resin, is a kind of porous polymeric polymer absorbant with good adsorbent function. It is with styrene and acrylate for monomer, addition divinylbenzene is cross-linking agent, with toluene, dimethylbenzene for porogen, they are cross-linked with each other to be polymerized and form porous skeleton structure, polymer removes porogen after being formed, then be internally formed at resin three-dimensional vary in size, different, the macroreticular structure that interpenetrates. Macroporous adsorbent resin has that cost is low, selectivity good, the big speed of adsorption capacity is fast, desorption mild condition and be prone to the plurality of advantages such as regeneration, and at normal temperatures insoluble in any solvent, stable in properties, in recent years, macroporous adsorbent resin has been widely used in the extraction research of Effective Component of Chinese Medicine, and studies effect and the prospect widely of thinking that macroporous adsorbent resin has uniqueness in chemical composition of Chinese materia medica separates.
High speed adverse current chromatogram (high-speedcountercurrentchromatography, HSCCC) it is novel liquid luquid partition chromatography technology, it utilizes multi-layer helix-tube synchronization line planetary centrifugal motion, realizing the sample efficient distribution in immiscible two-phase solvent system at short notice, separating thus realizing sample.Advantage maximum for HSCCC is in that each sample size is relatively larger, it is possible to reach a milligram magnitude, even gram quantity level; Meanwhile, HSCCC is DNAcarrier free separation, so being absent from the absorption of carrier, the utilization rate of sample is very high. HSCCC instrument price is cheap, dependable performance, analysis cost are low, easily operated, is a kind of modern equipment suitable in Chinese medicine and Natural products research. In view of the distinguishing feature of HSCCC, technique has been applied to the fields such as biochemistry, biological engineering, medicine, natural product chemistry, organic synthesis, environmental analysis, food, geology, material.
Summary of the invention
The present invention relates to a kind of method extracting high purity mangiferin from common bombax leaf, comprise the following steps:
(1) common bombax leaf is taken, drying, pulverization process, extract 1-3 time with the alcoholic solution of 8-20 times amount, each 20-60 minute. United extraction liquid, filters, and concentrating under reduced pressure obtains extractum, dries to obtain chimonin crude product.
(2) the chimonin crude product that step (1) obtains is dissolved in the alcoholic solution of 10%-30%, at 50 DEG C-100 DEG C, water-bath is extracted 1-3 time, united extraction liquid, filtering, filtrate is adjusted to loading AB-8 macroporous resin after PH1.0-5.0, loading flow velocity is 2BV/h, with the water elution remove impurity of 4BV after loading, then with 30%-50% alcoholic solution eluting, elution flow rate is 2BV/h, can't detect till chimonin in eluent. Collect whole eluent evaporated under reduced pressure.
(3) powder that step (2) obtains is further purified then through HSCCC. The solvent system of preparation ethyl acetate-n-butanol-water (4:1:5) or (3:2:5), fully shakes up rear stratification, and upper phase is fixing phase, and lower phase is mobile phase. After two-phase laminated flow, fix and pump into high-speed counter-current chromatograph with the flow velocity of 20ml/mim, after phase to be fixed is stable, regulates chromatograph and rotate with the speed of 800rpm, and mobile phase is pumped into the flow velocity of 2ml/min. Until in chromatograph biphase stable after, the mobile phase being mixed with sample is pumped into from sample port. Collecting each component according to the display of HSCCC collection of illustrative plates, and carry out HPLC detection, merged by the sample containing single chimonin, solvent evaporated obtains chimonin.
Preferably,
In described step (1), determining alcohol is 50%-80%, more preferably, and 70%;
In described step (1), alcoholic solution weight is 12 times amount, extracts 2 times, and extracting method uses hot reflux, ultrasonic or normal pressure diafiltration, it is preferred that, use ultrasonic extracting method;
In described step (1), extraction time is 20-40 minute, it is preferred that, extract 30 minutes;
In described step (2), being dissolved in 20% alcoholic solution by the chimonin crude product that step (1) obtains, at 75 DEG C, water-bath is extracted;
In described step (2), ethanol elution concentration is 50%;
In described step (3), ethyl acetate-n-butanol-water ratio is (4:1:5).
Compared with prior art, present invention have the advantage that
1. the present invention is with common bombax leaf for raw material, and it contains a large amount of chimonin, and raw material does not contain pesticide and noxious substance in process of production, and the chimonin quality prepared is high.
2. the solvent used in all processes of the present invention is nontoxic solvent, non-environmental-pollution, and Technology is reliable, and simple to operate, manpower and materials consumption is few, and cost is low.
3. having present invention firstly provides the method extracting high purity mangiferin from common bombax leaf in conjunction with macroporous resin and high speed adverse current chromatogram, result shows that the chimonin content obtained is high, is suitable for industrial mass production.
It is embodied as real formula
Referring to specific embodiment, the present invention is described. It will be appreciated by those skilled in the art that these embodiments are merely to illustrate the present invention, its scope not limited the present invention in any way.
Experimental technique in following embodiment, if no special instructions, is conventional method. Medicinal raw material used in following embodiment, reagent material etc., if no special instructions, be commercially available purchase product.
1 one kinds of methods extracting high purity mangiferin from common bombax leaf of embodiment
(1) take common bombax leaf 50g, drying, pulverization process, extract 2 times with 600ml70% alcoholic solution, each 30 minutes. United extraction liquid, filters, and concentrating under reduced pressure obtains extractum, dries to obtain chimonin crude product 4.7g.
(2) the chimonin crude product that step (1) obtains is dissolved in the alcoholic solution of 20%, at 75 DEG C, water-bath is extracted 2 times, united extraction liquid, filtering, filtrate is adjusted to loading AB-8 macroporous resin after PH4.0, loading flow velocity is 2BV/h, with the water elution remove impurity of 4BV after loading, then with 50% alcoholic solution eluting, elution flow rate is 2BV/h, can't detect till chimonin in eluent. Collect whole eluent, and evaporated under reduced pressure obtains powder 2.5g, chimonin purity >=50%.
(3) powder that step (2) obtains is further purified then through HSCCC. The solvent system of preparation ethyl acetate-n-butanol-water (4:1:5), fully shakes up rear stratification, and upper phase is fixing phase, and lower phase is mobile phase. After two-phase laminated flow, fix and pump into high-speed counter-current chromatograph with the flow velocity of 20ml/mim, after phase to be fixed is stable, regulates chromatograph and rotate with the speed of 800rpm, and mobile phase is pumped into the flow velocity of 2ml/min. Until in chromatograph biphase stable after, the mobile phase being mixed with sample is pumped into from sample port. Collecting each component according to the display of HSCCC collection of illustrative plates, and carry out HPLC detection, merged by the sample containing single chimonin, solvent evaporated obtains chimonin 46mg, chimonin purity >=98%.
2 one kinds of methods extracting high purity mangiferin from common bombax leaf of embodiment
(1) take common bombax leaf 50g, drying, pulverization process, extract 2 times with 400ml70% alcoholic solution, each 40 minutes. United extraction liquid, filters, and concentrating under reduced pressure obtains extractum, dries to obtain chimonin crude product 4.3g.
(2) the chimonin crude product that step (1) obtains is dissolved in the alcoholic solution of 10%, at 80 DEG C, water-bath is extracted 2 times, united extraction liquid, filtering, filtrate is adjusted to loading AB-8 macroporous resin after PH4.0, loading flow velocity is 2BV/h, with the water elution remove impurity of 4BV after loading, then with 30% alcoholic solution eluting, elution flow rate is 2BV/h, can't detect till chimonin in eluent. Collect whole eluent, and evaporated under reduced pressure obtains powder 2.0g, chimonin purity >=50%.
(3) powder that step (2) obtains is further purified then through HSCCC. The solvent system of preparation ethyl acetate-n-butanol-water (3:2:5), fully shakes up rear stratification, and upper phase is fixing phase, and lower phase is mobile phase. After two-phase laminated flow, fix and pump into high-speed counter-current chromatograph with the flow velocity of 20ml/mim, after phase to be fixed is stable, regulates chromatograph and rotate with the speed of 800rpm, and mobile phase is pumped into the flow velocity of 2ml/min. Until in chromatograph biphase stable after, the mobile phase being mixed with sample is pumped into from sample port. Collecting each component according to the display of HSCCC collection of illustrative plates, and carry out HPLC detection, merged by the sample containing single chimonin, solvent evaporated obtains chimonin 41mg, chimonin purity >=90%.
3 one kinds of methods extracting high purity mangiferin from common bombax leaf of embodiment
(1) take common bombax leaf 50g, drying, pulverization process, extract 2 times with 1000ml70% alcoholic solution, each 60 minutes. United extraction liquid, filters, and concentrating under reduced pressure obtains extractum, dries to obtain chimonin crude product 4.9g.
(2) the chimonin crude product that step (1) obtains is dissolved in the alcoholic solution of 30%, at 100 DEG C, water-bath is extracted 2 times, united extraction liquid, filtering, filtrate is adjusted to loading AB-8 macroporous resin after PH4.0, loading flow velocity is 2BV/h, with the water elution remove impurity of 4BV after loading, then with 40% alcoholic solution eluting, elution flow rate is 2BV/h, can't detect till chimonin in eluent. Collect whole eluent, and evaporated under reduced pressure obtains powder 2.7g, chimonin purity >=50%.
(3) powder that step (2) obtains is further purified then through HSCCC. The solvent system of preparation ethyl acetate-n-butanol-water (4:1:5), fully shakes up rear stratification, and upper phase is fixing phase, and lower phase is mobile phase. After two-phase laminated flow, fix and pump into high-speed counter-current chromatograph with the flow velocity of 20ml/mim, after phase to be fixed is stable, regulates chromatograph and rotate with the speed of 800rpm, and mobile phase is pumped into the flow velocity of 2ml/min. Until in chromatograph biphase stable after, the mobile phase being mixed with sample is pumped into from sample port. Collecting each component according to the display of HSCCC collection of illustrative plates, and carry out HPLC detection, merged by the sample containing single chimonin, solvent evaporated obtains chimonin 45mg, chimonin purity >=95%.
Claims (8)
1. the method extracting high purity mangiferin from common bombax leaf, it is characterised in that described extracting method comprises the following steps:
(1) common bombax leaf is taken, drying, pulverization process, extract 1-3 time with the alcoholic solution of 8-20 times amount, each 20-60 minute; United extraction liquid, filters, and concentrating under reduced pressure obtains extractum, dries to obtain chimonin crude product;
(2) the chimonin crude product that step (1) obtains is dissolved in the alcoholic solution of 10%-30%, at 50 DEG C-100 DEG C, water-bath is extracted 1-3 time, united extraction liquid, filtering, filtrate is adjusted to loading AB-8 macroporous resin after PH1.0-5.0, loading flow velocity is 2BV/h, with the water elution remove impurity of 4BV after loading, then with 30%-50% alcoholic solution eluting, elution flow rate is 2BV/h, can't detect till chimonin in eluent; Collect whole eluent evaporated under reduced pressure;
(3) powder that step (2) obtains is further purified then through HSCCC, the solvent system of preparation ethyl acetate-n-butanol-water (4:1:5) or (3:2:5), fully shaking up rear stratification, upper phase is fixing phase, and lower phase is mobile phase; After two-phase laminated flow, fix and pump into high-speed counter-current chromatograph with the flow velocity of 20ml/mim, after phase to be fixed is stable, regulates chromatograph and rotate with the speed of 800rpm, and mobile phase is pumped into the flow velocity of 2ml/min; Until in chromatograph biphase stable after, the mobile phase being mixed with sample is pumped into from sample port; Collecting each component according to the display of HSCCC collection of illustrative plates, and carry out HPLC detection, merged by the sample containing single chimonin, solvent evaporated obtains chimonin.
2. a kind of method extracting high purity mangiferin from common bombax leaf according to claim 1, it is characterised in that step (1) described determining alcohol is 50%-80%, more preferably, 70%.
3. a kind of method extracting high purity mangiferin from common bombax leaf according to claim 1, it is characterized in that, the described alcoholic solution weight of step (1) is for for 12 times amount, extract 2 times, extracting method uses hot reflux, ultrasonic or normal pressure diafiltration, it is preferred that, use ultrasonic extracting method.
4. a kind of method extracting high purity mangiferin from common bombax leaf according to claim 1, it is characterised in that step (1) described extraction time is 20-40 minute, it is preferred that, extract 30 minutes.
5. a kind of method extracting high purity mangiferin from common bombax leaf according to claim 1, it is characterized in that, in described step (2), being dissolved in 20% alcoholic solution by the chimonin crude product that step (1) obtains, at 75 DEG C, water-bath is extracted.
6. a kind of method extracting high purity mangiferin from common bombax leaf according to claim 1, it is characterised in that in described step (2), ethanol elution concentration is 50%.
7. a kind of method extracting high purity mangiferin from common bombax leaf according to claim 1, it is characterised in that in described step (3), ethyl acetate-n-butanol-water ratio is (4:1:5).
8. the method extracting high purity mangiferin from common bombax leaf, it is characterised in that described extracting method comprises the following steps:
(1) common bombax leaf is taken, drying, pulverization process, extract 2 times with the alcoholic solution of 12 times amount, each 30 minutes; United extraction liquid, filters, and concentrating under reduced pressure obtains extractum, dries to obtain chimonin crude product;
(2) the chimonin crude product that step (1) obtains is dissolved in the alcoholic solution of 20%, at 75 DEG C, water-bath is extracted 1-3 time, united extraction liquid, filtering, filtrate is adjusted to loading AB-8 macroporous resin after PH1.0-5.0, loading flow velocity is 2BV/h, with the water elution remove impurity of 4BV after loading, then with 50% alcoholic solution eluting, elution flow rate is 2BV/h, can't detect till chimonin in eluent; Collect whole eluent evaporated under reduced pressure;
(3) powder that step (2) obtains is further purified then through HSCCC; The solvent system of preparation ethyl acetate-n-butanol-water (4:1:5), fully shakes up rear stratification, and upper phase is fixing phase, and lower phase is mobile phase; After two-phase laminated flow, fix and pump into high-speed counter-current chromatograph with the flow velocity of 20ml/mim, after phase to be fixed is stable, regulates chromatograph and rotate with the speed of 800rpm, and mobile phase is pumped into the flow velocity of 2ml/min; Until in chromatograph biphase stable after, the mobile phase being mixed with sample is pumped into from sample port; Collecting each component according to the display of HSCCC collection of illustrative plates, and carry out HPLC detection, merged by the sample containing single chimonin, solvent evaporated obtains chimonin.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110146622A (en) * | 2019-06-13 | 2019-08-20 | 青海省药品检验检测院 | The measuring method and quality assessment method of mangiferin in a kind of common bombax flower |
| CN111012705A (en) * | 2019-12-18 | 2020-04-17 | 广州市巧美化妆品有限公司 | Extraction process of kapok leaf extract and essence cream thereof |
| CN113846330A (en) * | 2021-09-28 | 2021-12-28 | 广州大学 | Plant compound corrosion inhibitor and preparation method and application thereof |
-
2016
- 2016-02-23 CN CN201610099728.3A patent/CN105646464A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110146622A (en) * | 2019-06-13 | 2019-08-20 | 青海省药品检验检测院 | The measuring method and quality assessment method of mangiferin in a kind of common bombax flower |
| CN111012705A (en) * | 2019-12-18 | 2020-04-17 | 广州市巧美化妆品有限公司 | Extraction process of kapok leaf extract and essence cream thereof |
| CN113846330A (en) * | 2021-09-28 | 2021-12-28 | 广州大学 | Plant compound corrosion inhibitor and preparation method and application thereof |
| CN113846330B (en) * | 2021-09-28 | 2023-09-01 | 广州大学 | Plant compound corrosion inhibitor and preparation method and application thereof |
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