CN1166679C - Method for extracting and separating notoginsenoside R1, panaxcoside Re, pseudo-ginseng element from pseudo-ginseng crude powder - Google Patents
Method for extracting and separating notoginsenoside R1, panaxcoside Re, pseudo-ginseng element from pseudo-ginseng crude powder Download PDFInfo
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- CN1166679C CN1166679C CNB011366974A CN01136697A CN1166679C CN 1166679 C CN1166679 C CN 1166679C CN B011366974 A CNB011366974 A CN B011366974A CN 01136697 A CN01136697 A CN 01136697A CN 1166679 C CN1166679 C CN 1166679C
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- arasaponin
- dencichine
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Abstract
The present invention relates to a method for extracting and separating arasaponin R1, ginsenoside Re and dencichine from notoginseng raw powder. The present invention comprises the following procedures: methanol extract and residues are obtained by leaching notoginseng raw powder by methanol, and methanolic extract is obtained by concentrating and drying methanol extract; water is added to the methanolic extract, and extraction is carried out by petroleum ether to obtain water phases; extraction is carried out by normal butyl alcohol to obtain normal butyl alcohol phases, and arasaponin crude extract is obtained after the normal butyl alcohol phases are steamed and dried, arasaponin R1 and ginsenoside Re are obtained by separating the arasaponin crude extract, and the residues of the notoginseng raw powder are extracted by water after methanol extraction to obtain water extract; the water extract is extracted by normal butyl alcohol, water layers are freeze-dried to obtain dencichine crude extract, and the dencichine crude extract is further separated and purified to obtain notoginseng. The method has the advantage of simple and novel operation.
Description
Technical field
The present invention relates to a kind of from pseudo-ginseng fecula extraction separation arasaponin R
1, ginsenoside Re, dencichine method.
Background technology
Pseudo-ginseng is a kind of traditional rare traditional Chinese medicine of China, it has effects such as hemostasia and dissipation blood stasis, swelling and pain relieving, the wound of living, pharmacological research in recent years shows, pseudo-ginseng also has coronary blood flow increasing, reduce the effect of myocardial consumption of oxygen and arteriotony, be used for the treatment of coronary heart disease, stenocardia acquisition significant curative effect.Main active ingredient saponin class in the pseudo-ginseng, wherein arasaponin R
1Be its endemic element; Radix Notoginseng total arasaponins has been used for the treatment of migraine clinically; calm; sleep peacefully and anti inflammation and heat resolution etc.; arasaponin structurally is dammarane's tetracyclic triterpene type saponin; in addition; also containing a kind of activeconstituents in the pseudo-ginseng is dencichine; studies show that; it is the main hemostatic compositions in the pseudo-ginseng; its structure is β-N-oxalic acid-acyl group-L-α; β-diaminopropionic acid; up to the present; on market, almost can not find arasaponin and pure product of dencichine and reference substance; and because the special chemical property of arasaponin; no uv-absorbing, and dencichine is a kind of special amino acid has higher economic value and learning value to the research and development of its extraction and separation method.
Summary of the invention
The purpose of this invention is to provide a kind of from pseudo-ginseng fecula extraction separation arasaponin R
1, ginsenoside Re, dencichine method, this method is simple to operate, novel.
For achieving the above object, the present invention takes following design: a kind of from pseudo-ginseng fecula extraction separation arasaponin R
1, ginsenoside Re, dencichine method, it is characterized in that: it may further comprise the steps: the pseudo-ginseng fecula is with the methyl alcohol lixiviate, methanol extract liquid and residue, with the methanol extract liquid concentrate drying, obtain methanol extract, methanol extract adds water, and with petroleum ether extraction, the water intaking phase, with n-butanol extraction, get the propyl carbinol phase, behind the evaporate to dryness, the arasaponin crude extract, this saponin crude extract separate arasaponin R
1And ginsenoside Re; Pseudo-ginseng fecula residue obtains water extract with water extraction behind the methanol extraction, and water extract gets the dencichine crude extract with n-butanol extraction with the water layer lyophilize, and the further separation and purification of dencichine crude extract gets pseudo-ginseng.
Description of drawings
Fig. 1 separates the arasaponin R that obtains for utilizing the HSCCC the first step among the present invention
1Thin-layer chromatogram with the ginsenoside Re mixture
Fig. 2 is the high-efficient liquid phase chromatogram of mixture among Fig. 1
Fig. 3 separates the thin-layer chromatogram of two kinds of saponins that obtain for utilizing second step of HSCCC in the invention
Fig. 4 A, Fig. 4 B are that the second step HSCCC separates a kind of saponin liquid chromatogram (203nm) (16 pipes, 15 pipes) that obtains
Fig. 5 A, Fig. 5 B are that the second step HSCCC separates the another kind of saponin color atlas (203nm) (17 pipes, 18 pipes) that obtains
Embodiment
Embodiment 1
One, takes by weighing Radix Notoginseng powder 100g and add 500ml methyl alcohol, soaked 36 hours, after the filtration, the filtrate evaporate to dryness is got methanol extract.After this methanol extract usefulness distilled water 300ml dissolving, earlier, discard phase, take off layer water with twice of isopyknic n-butanol extraction with isopyknic sherwood oil (boiling range is 60-90 ℃) extracting twice, the gained propyl carbinol is merged evaporate to dryness mutually, get 10.2g arasaponin crude extract.
Two, utilize high speed adverse current chromatogram (HSCCC) the first step to separate and obtain arasaponin R
1, ginsenoside Re mixture.
1, adopts chloroform, methyl alcohol, propyl alcohol, aqueous systems, wherein chloroform: methyl alcohol: propyl alcohol: water=6: 6: 1: 4 (volume ratios)
Get the arasaponin crude extract, its applied sample amount 200mg, column volume 200ml, main frame revolution 800rpm, on the phase that fixes mutually, make moving phase, flow rate of mobile phase 2ml/min down mutually.
2, operation steps: than the preparation solvent system, standing demix in separating funnel is told phase up and down by each solvent volume, on fix mutually phase, down make moving phase mutually, make to be full of stationary phase in the counter current chromatograph pillar, its main frame is rotated, again moving phase is pumped in the post, by the sampling valve sample introduction.(this separation adopts the counter current chromatograph of New Technique Application Inst., Beijing City development to finish.)
Because arasaponin R
1Reaching ginsenoside Re does not have uv-absorbing, so the conventional UV-detector that can't use high-speed counter-current chromatograph (HSCCC) to be joined detects peak and separation case.Therefore, adopting automatically in this experiment, collection divides collector, setting-up time, each fraction under the wash-out behind the sample on the Fractional Collections high-speed counter-current chromatograph.Each is inhaled and to be in charge of with the thin-layer chromatography check and analysis then, adopts the unfolding condition identical with pharmacopeia, by with pharmacopeia in the spectrogram comparison is provided.Collection contains arasaponin R
1Its thin-layer developing spectrogram as shown in Figure 1 with the fraction (25-38 pipe) of ginsenoside Re.
By above separation, can get arasaponin R
1And ginsenoside Re mixture 13mg.Its efficient liquid phase chromatographic analysis spectrum is seen shown in Figure 2.
Three, the mixture that above-mentioned separation obtains is further separated (second step separated) with high-speed counter-current chromatograph
1, adopt ethyl acetate: propyl carbinol: water=2: 1: 3 volume ratios, applied sample amount are the first step separating for several times products therefrom 40mg altogether, column volume 200m1, main frame revolution 800rpm.On the phase that fixes mutually, make moving phase, flow rate of mobile phase 2ml/min down mutually.
2, operation steps is the same, divides collector to collect with collection, the lease making thin-layer chromatography at different levels check and analysis of wash-out and with pharmacopeia in provide spectrogram relatively, keep and contain arasaponin R
1With fraction (15-18) pipe of ginsenoside Re, its thin-layer developing figure sees shown in Figure 3.
3, see Fig. 4 A, Fig. 4 B through high performance liquid chromatography check and analysis the 15th to 16 pipe for a kind of saponin (24mg), the 17-18 pipe is seen Fig. 5 A, Fig. 5 B for another saponin (13mg), and both separate fully.
(present embodiment system extracts dencichine to embodiment 2 from the residual residue behind the pseudo-ginseng fecula methanol extraction
Embodiment).
Extraction step: the residue of pseudo-ginseng fecula behind methanol extraction, use water extraction, the gained water extract, through n-butanol extraction, water through lyophilize get final product the dencichine crude extract, 100g pseudo-ginseng fecula can get the about 10g of dencichine crude extract, wherein mainly contains several aminoacid components such as dencichine and arginine through amino acid analysis.The dencichine crude extract separates with the gel chromatographic columns of Sephadex LH-20, with sample on 1/10 the ratio of column packing, the deionized water wash-out, collect each fraction with run tank, point sample is analyzed with ninhydrin respectively, can with ninhydrin reaction, manifest mauve fraction, use paper chromatography point sample, triketohydrindene hydrate chromogenic assay more respectively.Merge the level lease making lyophilize that contains dencichine and get intermediate product.This product process CMSephadex C-25 is chromatographic separation once more, adopts same methods analyst, collects the target fraction, lyophilize.In case of necessity, can carry out multiple CM-Sephadex C25 post and separate or recrystallization, can obtain the pure product of dencichine.
The analytical procedure of dencichine:
1, amino acidanalyser autoanalyzer method
Chromatography column: 4.6 * 150mm Zeo-karb
Damping fluid flow velocity: 0.425ml/min
Column temperature: 50 ℃, sample size: 50 μ l, analysis time 50min.
2, ply of paper is analysed a ninhydrin
Upholder: chromatography filter paper
Developping agent: propyl carbinol-acetate-water-dehydrated alcohol (4: 1: 2: 1)
Development process: behind the 1% triketohydrindene hydrate aqueous solution of spraying, heating 3 minutes is displaing amaranth, and this method is amino acid whose feature coloration method, the shift value Rf=0.1 of dencichine.
Advantage of the present invention: can obtain respectively the product of purifying in the method provided by the invention, and method is easy, The gained sterling is through assert standard items or the reference substance that can be used as quality control, and is very with practical value.
Claims (1)
1, a kind of from pseudo-ginseng fecula extraction separation arasaponin R
1, ginsenoside Re, dencichine method, it is characterized in that: it may further comprise the steps: the pseudo-ginseng fecula is with the methyl alcohol lixiviate, methanol extract liquid and residue, with the methanol extract liquid concentrate drying, obtain methanol extract, methanol extract adds water, and with petroleum ether extraction, the water intaking phase, with n-butanol extraction, get the propyl carbinol phase, behind the evaporate to dryness, the arasaponin crude extract, this saponin crude extract separate arasaponin R
1And ginsenoside Re, it is to adopt the high speed adverse current chromatogram method that described thick arasaponin separates, and collects respectively and respectively separates fraction, check and analysis get arasaponin R
1Mixture with ginsenoside Re, one's duty exsolution agent system is chloroform, methyl alcohol, propyl alcohol, water, each volume ratio is 6: 6: 1 in described chloroform, methyl alcohol, propyl alcohol, the aqueous systems: 4, on fix mutually phase, down do moving phase mutually, use high speed adverse current chromatogram and further separate said mixture, obtain arasaponin R respectively
1And ginsenoside Re, its solvent for use system consists of ethyl acetate, propyl carbinol, water, and volume ratio is an ethyl acetate in the described further separatory solvent system: propyl carbinol: water=2: 1: 3; Pseudo-ginseng fecula residue is with water extraction behind the methanol extraction, obtain water extract, water extract is with n-butanol extraction, the water layer lyophilize is got the dencichine crude extract, the further separation and purification of dencichine crude extract gets dencichine, described dencichine crude extract separation purification method is that the dencichine crude extract is separated with gel chromatographic columns Sephadex Lh-20, use the deionized water wash-out, collection can with triketohydrindene hydrate generation color reaction component, point sample is analysed-the ninhydrin analysis with ply of paper respectively, merges to contain the dencichine component, get intermediate product through lyophilize, product is once more with CM SephadexC-25 chromatographic separation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011366974A CN1166679C (en) | 2001-10-26 | 2001-10-26 | Method for extracting and separating notoginsenoside R1, panaxcoside Re, pseudo-ginseng element from pseudo-ginseng crude powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011366974A CN1166679C (en) | 2001-10-26 | 2001-10-26 | Method for extracting and separating notoginsenoside R1, panaxcoside Re, pseudo-ginseng element from pseudo-ginseng crude powder |
Publications (2)
| Publication Number | Publication Date |
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| CN1414009A CN1414009A (en) | 2003-04-30 |
| CN1166679C true CN1166679C (en) | 2004-09-15 |
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| CNB011366974A Expired - Fee Related CN1166679C (en) | 2001-10-26 | 2001-10-26 | Method for extracting and separating notoginsenoside R1, panaxcoside Re, pseudo-ginseng element from pseudo-ginseng crude powder |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1771978B (en) * | 2004-11-09 | 2011-06-08 | 成都华神集团股份有限公司制药厂 | Notoginseng triol-saponin composition and its preparation and use |
| CN100336801C (en) * | 2006-06-22 | 2007-09-12 | 上海交通大学 | Method for extracting notoginseng essence from notoginseng |
| CN103193846B (en) * | 2013-04-01 | 2015-01-14 | 中国药科大学 | Preparation method of cis-trans isomers of ginsenoside Rk3 and ginsenoside Rh4 |
| CN104774237B (en) * | 2014-01-09 | 2017-10-13 | 天津天士力之骄药业有限公司 | A kind of Panax zingiberensis C.Y.Wu. Et Feng saponin(e R1 preparation method |
| CN103919795B (en) * | 2014-03-30 | 2015-11-18 | 吴静 | A kind of containing dencichine and arasaponin R1 pharmaceutical composition and preparation thereof |
| CN107970265B (en) * | 2017-12-28 | 2021-05-04 | 云南汉德生物技术有限公司 | Method for extracting sanchinoside |
| CN115453035A (en) * | 2022-10-18 | 2022-12-09 | 湖南祥民制药有限公司 | Method for extracting high-content notoginsenoside R1 from panax notoginseng |
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