CN102649807A - Preparation method of Heteropappus altaicus saponin (I) - Google Patents
Preparation method of Heteropappus altaicus saponin (I) Download PDFInfo
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- CN102649807A CN102649807A CN201110045314XA CN201110045314A CN102649807A CN 102649807 A CN102649807 A CN 102649807A CN 201110045314X A CN201110045314X A CN 201110045314XA CN 201110045314 A CN201110045314 A CN 201110045314A CN 102649807 A CN102649807 A CN 102649807A
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Abstract
The invention relates to a preparation method of a Heteropappus altaicus saponin (I). The method comprises the following steps of: smashing Heteropappus altaicu herb utilized as a water material, extracting with an ethanol water, leaching an extracting solution, concentrating under reduced pressure until no alcohol exists, dispersing in water, and separating a dispersing solution by utilizing a macroporous resin column and prepared high-liquid chromatography sequentially so as to prepare the high-purity Heteropappus altaicus saponin (I). The preparation method has the advantages that the process is stable, the content of the product Heteropappus altaicus saponin (I) is high and can reach above 98%.
Description
Technical field:
The present invention relates to the preparation method of a kind of dog flower saponin(e (I), be specifically related to a kind ofly use that post separates and the method for high liquid phase production fast.
Background technology:
Altay dog flower (Heteropappus altaicus (Willd.) Novopokr.) has another name called Herba Heteropappi Altaici, is composite family dog flower plant; Herb or root are gone into Chinese medicine; Extensively be born in grassland and meadow steppe band, also be born near mountain region, hills, roadside, the cottage, output is extremely many.Altay dog flower is distributed in ground (district) such as China northeast, North China, the Inner Mongol, Shaanxi, Hubei, Sichuan, Gansu, Qinghai, Xinjiang, Tibet; Also there are distribution in Mongolia, the Soviet Union (siberian and Central Asia).All herbal medicine can be clearing heat and detoxicating, apocenosis, moistening lung sending down abnormally ascending, preventing phlegm from forming and stopping coughing, diuresis.Cure mainly the epidemic disease pyreticosis, high heat headache, hepatobiliary hyperactivity, fullness in the chest and hypochondrium is vexed, irritated irritability, carbuncle sore furuncle, venom, the cough due to deficiency of the lung, spitting of blood, chronic bronchitis, gonorrhoea, dysuria is controlled pestilence, and blood-head is scorchingly hot, seasonal febrile diseases, diseases such as measles without adequate eruption.
Altay dog flower composition is mainly essential oil, flavonoid, triterpene saponin, and main saponin constituent is a A Erai dog flower saponin(e (I), is the oleanane type saponin(e, has antimycotic, antitumor and the adjusting immunocompetence.
The preparation method of the Altay dog flower saponin(e that is up to the present adopted has plenty of raw material is extracted n-butanol extraction with aqueous ethanolic solution heat; The impurity that extracts is more; Be unfavorable for the monomeric separation of dog flower saponin(e (I), what have will be through silica gel column chromatography repeatedly, has not only taken solvent but also time-consuming; Productive rate is low, and cost is higher.At present, the high performance liquid preparative chromatography work that is used for the high-load dog of mass preparation flower saponin(e (I) does not also appear in the newspapers.
Summary of the invention:
The preparation method who the purpose of this invention is to provide a kind of dog flower saponin(e (I).This method can realize the preparation of high purity dog flower saponin(e (I).
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
The preparation method of a kind of dog flower saponin(e (I) is characterized in that comprising the steps: Altay dog flower herb is pulverized, and extracts 1-4 time each 0.5-4h with aqueous ethanolic solution; Suction filtration, merging filtrate, concentrating under reduced pressure does not have alcohol; Be scattered in the water, through macroporous resin column, it is colourless that water is washed till water lotion earlier for dispersion liquid; Washing lotion discards, and uses the 50-80% ethanol elution again, collects elutriant; Concentrating under reduced pressure, the dry powder that gets adopt preparation type high liquid chromatography to separate the highly purified dog flower of preparation saponin(e (I) again, and the content of measuring product dog flower saponin(e (I) through HPLC is more than 98%.
Said aqueous ethanolic solution volume percent is 60-80%, and process for extracting is a kind of in microwave-assisted extraction, heating and refluxing extraction or the supersound extraction.
The optional AB-8 of said macroporous resin model, LSA-21, HPD-400 etc.
Beneficial effect of the present invention is:
(1) integrated artistic of the present invention is simple to operate, and feasibility is strong;
(2) the present invention is a separation means with the high liquid phase of preparation type, can obtain purity at the flower of the dog more than 98% saponin(e (I), and the single needle disengaging time is short, is fit to very much large batch of preparation, prepares the recyclable utilization of solvent simultaneously, can realize batch preparations;
(3) the present invention uses the macroporous resin removal of impurities earlier before the preparation high liquid chromatography, can prolong the work-ing life of chromatographic column.
Combine embodiment that the present invention is further specified, embodiment only limits to explain the present invention at present, but not to qualification of the present invention.
Embodiment:
Embodiment 1:
Altay dog Hua Quange is pulverized, get 1kg, with 80% aqueous ethanolic solution heating and refluxing extraction 4 times, 0.5h at every turn; Suction filtration, merging filtrate, concentrating under reduced pressure does not have alcohol, is scattered in the water; Through the LSA-21 macroporous resin column, it is colourless that water is washed till water lotion earlier for dispersion liquid, and washing lotion discards, and uses the 4L60% ethanol elution again; Collect elutriant, concentrating under reduced pressure, the dry powder that gets with the dissolving of 75% second, are made into the solution that concentration is 50mg/ml; Through 0.45 μ m micro-filtrate membrane filtration, preparation type high liquid chromatography preparative column is a filler with the C8 bonding mutually, and particle diameter is 10 μ m, and column length is that 15cm, diameter are 7cm; Six-way valve sample introduction, sampling volume are 25ml, and the acetonitrile solution with 45% is a moving phase, and the control flow velocity is 50ml/min; On-line ultraviolet detects, and collects the high purity flow point that contains dog flower saponin(e (I), is concentrated into to do that promptly get content be that 98.26% dog is spent saponin(e (I).
Embodiment 2:
Altay dog flower herb is pulverized, got 1kg, with 70% aqueous ethanolic solution supersound extraction 1 time, 4h at every turn; Suction filtration, merging filtrate, concentrating under reduced pressure does not have alcohol, is scattered in the water; Through the AB-8 macroporous resin column, it is colourless that water is washed till water lotion earlier for dispersion liquid, and washing lotion discards, and uses the 5L70% ethanol elution again; Collect elutriant, concentrating under reduced pressure, the dry powder that gets with the dissolving of 75% second, are made into the solution that concentration is 100mg/ml; Through 0.45 μ m micro-filtrate membrane filtration, preparation type high liquid chromatography preparative column is a filler with the C18 bonding mutually, and particle diameter is 20 μ m, and column length is that 10cm, diameter are 1cm; Six-way valve sample introduction, sampling volume are 5ml, and the acetonitrile solution with 35% is a moving phase, and the control flow velocity is 10ml/min; On-line ultraviolet detects, and collects the high purity flow point that contains dog flower saponin(e (I), is concentrated into to do that promptly get content be that 98.89% dog is spent saponin(e (I).
Embodiment 3:
Altay dog flower herb is pulverized, got 1kg, extract 3 times, each 1.5h with 60% aqueous ethanolic solution microwave-assisted; Suction filtration, merging filtrate, concentrating under reduced pressure does not have alcohol, is scattered in the water; Through the AB-8 macroporous resin column, it is colourless that water is washed till water lotion earlier for dispersion liquid, and washing lotion discards, and uses the 5L50% ethanol elution again; Collect elutriant, concentrating under reduced pressure, the dry powder that gets with the dissolving of 75% second, are made into the solution that concentration is 80mg/ml; Through 0.45 μ m micro-filtrate membrane filtration, preparation type high liquid chromatography preparative column is a filler with the C18 bonding mutually, and particle diameter is 15 μ m, and column length is that 50cm, diameter are 10cm; Six-way valve sample introduction, sampling volume are 30ml, and the acetonitrile solution with 55% is a moving phase, and the control flow velocity is 250ml/min; On-line ultraviolet detects, and collects the high purity flow point that contains dog flower saponin(e (I), is concentrated into to do that promptly get content be that 99.22% dog is spent saponin(e (I).
Embodiment 4:
Altay dog flower herb is pulverized, got 2kg, with 75% aqueous ethanolic solution heating and refluxing extraction 2 times, 2h at every turn; Suction filtration, merging filtrate, concentrating under reduced pressure does not have alcohol, is scattered in the water; Through the AB-8 macroporous resin column, it is colourless that water is washed till water lotion earlier for dispersion liquid, and washing lotion discards, and uses the 10L65% ethanol elution again; Collect elutriant, concentrating under reduced pressure, the dry powder that gets with the dissolving of 75% second, are made into the solution that concentration is 120mg/ml; Through 0.45 μ m micro-filtrate membrane filtration, preparation type high liquid chromatography preparative column is a filler with the C18 bonding mutually, and particle diameter is 5 μ m, and column length is that 40cm, diameter are 6cm; Six-way valve sample introduction, sampling volume are 50ml, and the acetonitrile solution with 40% is a moving phase, and the control flow velocity is 300ml/min; On-line ultraviolet detects, and collects the high purity flow point that contains dog flower saponin(e (I), is concentrated into to do that promptly get content be that 98.91% dog is spent saponin(e (I).
Embodiment 5:
Altay dog flower herb is pulverized, got 2kg, with 70% aqueous ethanolic solution supersound extraction 2 times, 3h at every turn; Suction filtration, merging filtrate, concentrating under reduced pressure does not have alcohol, is scattered in the water; Through the LSA-21 macroporous resin column, it is colourless that water is washed till water lotion earlier for dispersion liquid, and washing lotion discards, and uses the 10L80% ethanol elution again; Collect elutriant, concentrating under reduced pressure, the dry powder that gets with the dissolving of 75% second, are made into the solution that concentration is 100mg/ml; Through 0.45 μ m micro-filtrate membrane filtration, preparation type high liquid chromatography preparative column is a filler with the C18 bonding mutually, and particle diameter is 10 μ m, and column length is that 45cm, diameter are 4cm; Six-way valve sample introduction, sampling volume are 40ml, and the acetonitrile solution with 35% is a moving phase, and the control flow velocity is 350ml/min; On-line ultraviolet detects, and collects the high purity flow point that contains dog flower saponin(e (I), is concentrated into to do that promptly get content be that 99.03% dog is spent saponin(e (I).
Claims (3)
1. the preparation method of a dog flower saponin(e (I) is characterized in that comprising the steps: Altay dog flower herb is pulverized, and extracts 1-4 time each 0.5-4h with aqueous ethanolic solution; Suction filtration, merging filtrate, concentrating under reduced pressure does not have alcohol; Be scattered in the water, through macroporous resin column, it is colourless that water is washed till water lotion earlier for dispersion liquid; Washing lotion discards, and uses the 50-80% ethanol elution again, collects elutriant; Concentrating under reduced pressure, the dry powder that gets adopt preparation type high liquid chromatography to separate the highly purified dog flower of preparation saponin(e (I) again, and the content of measuring product dog flower saponin(e (I) through HPLC is more than 98%.
2. according to the preparation method of the said a kind of dog flower saponin(e of claim 1 (I), it is characterized in that said aqueous ethanolic solution volume percent is 60-80%, process for extracting is a kind of in microwave-assisted extraction, heating and refluxing extraction or the supersound extraction.
3. according to the preparation method of the said a kind of dog flower saponin(e of claim 1 (I), it is characterized in that the optional AB-8 of said macroporous resin model, LSA-21, HPD-400 etc.
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| CN201110045314XA CN102649807A (en) | 2011-02-25 | 2011-02-25 | Preparation method of Heteropappus altaicus saponin (I) |
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| CN201110045314XA CN102649807A (en) | 2011-02-25 | 2011-02-25 | Preparation method of Heteropappus altaicus saponin (I) |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103720735A (en) * | 2013-12-10 | 2014-04-16 | 内蒙古医科大学 | Application of heteropappus meyendorffii head flocculate |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010056181A1 (en) * | 1998-04-17 | 2001-12-27 | Alister D. Muir | Process for recovery and purification of saponins and sapogenins from quinoa (chenopodium quinoa) |
| US20040067263A1 (en) * | 2001-01-16 | 2004-04-08 | Dayou Liu | Method for preparating an anemone raddeana extract and the pharmaceutical composition containing the same as well as use thereof |
| CN101037465A (en) * | 2006-03-15 | 2007-09-19 | 北京同仁堂股份有限公司 | Steroid saponins and preparation method and application |
| CN101200487A (en) * | 2007-11-27 | 2008-06-18 | 浙江大学 | Method for preparing asiatic centella total saponins by using macroporous adsorption resin |
| CN101284861A (en) * | 2008-05-04 | 2008-10-15 | 天津大学 | Triterpenoid saponin compounds, preparation method and use |
| CN101899082A (en) * | 2010-07-22 | 2010-12-01 | 中南民族大学 | Triterpenoid saponin compound, application and preparation method |
| CN101906129A (en) * | 2010-07-29 | 2010-12-08 | 韶关学院 | Method for separating purified saponin |
-
2011
- 2011-02-25 CN CN201110045314XA patent/CN102649807A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010056181A1 (en) * | 1998-04-17 | 2001-12-27 | Alister D. Muir | Process for recovery and purification of saponins and sapogenins from quinoa (chenopodium quinoa) |
| US20040067263A1 (en) * | 2001-01-16 | 2004-04-08 | Dayou Liu | Method for preparating an anemone raddeana extract and the pharmaceutical composition containing the same as well as use thereof |
| CN101037465A (en) * | 2006-03-15 | 2007-09-19 | 北京同仁堂股份有限公司 | Steroid saponins and preparation method and application |
| CN101200487A (en) * | 2007-11-27 | 2008-06-18 | 浙江大学 | Method for preparing asiatic centella total saponins by using macroporous adsorption resin |
| CN101284861A (en) * | 2008-05-04 | 2008-10-15 | 天津大学 | Triterpenoid saponin compounds, preparation method and use |
| CN101899082A (en) * | 2010-07-22 | 2010-12-01 | 中南民族大学 | Triterpenoid saponin compound, application and preparation method |
| CN101906129A (en) * | 2010-07-29 | 2010-12-08 | 韶关学院 | Method for separating purified saponin |
Non-Patent Citations (2)
| Title |
|---|
| YU-LIN FENG,ET AL.: "thiterpenoidal saponins from the barks of zygophyllum fabago l.", 《CHEM. PHARM.BULL》 * |
| 杨淑敏等: "阿尔泰狗哇花总皂苷的提取与纯化", 《化学研究》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103720735A (en) * | 2013-12-10 | 2014-04-16 | 内蒙古医科大学 | Application of heteropappus meyendorffii head flocculate |
| CN103720735B (en) * | 2013-12-10 | 2017-01-11 | 内蒙古医科大学 | Application of heteropappus meyendorffii head flocculate |
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Application publication date: 20120829 |