CN102228486A - Preparation method for Pouzolzia zeylanica (L.) Benn. var. microphylla (Wedd.) W. T. Wang flavonoid - Google Patents
Preparation method for Pouzolzia zeylanica (L.) Benn. var. microphylla (Wedd.) W. T. Wang flavonoid Download PDFInfo
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- CN102228486A CN102228486A CN2011101179195A CN201110117919A CN102228486A CN 102228486 A CN102228486 A CN 102228486A CN 2011101179195 A CN2011101179195 A CN 2011101179195A CN 201110117919 A CN201110117919 A CN 201110117919A CN 102228486 A CN102228486 A CN 102228486A
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Abstract
The invention relates to a preparation method for Pouzolzia zeylanica (L.) Benn. var. microphylla (Wedd.) W. T. Wang flavonoids. The method comprises the following steps: using Pouzolzia zeylanica (L.) Benn. var. microphylla (Wedd.) W. T. Wang as a raw material, carrying out hot extraction with petroleum ether having a boiling range of 60 to 90 DEG C, carrying out extraction with an ethanol solution having a concentration of 50 to 70% twice to three times, condensing the extracts to form an extractum, adding acid water to disperse the extractum, carrying out filtering to obtain insoluble substances, and separating the insoluble substances with a macroporous resin to obtain Pouzolzia zeylanica (L.) Benn. var. microphylla (Wedd.) W. T. Wang flavonoids. The content of flavone in the obtained flavonoids is as much as 65 to 85%. The method provided in the invention has a simple process and produces a product with high purity.
Description
Technical field:
The invention belongs to natural drug extractive technique field, relate to a kind of preparation method of Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang total flavones.
Background technology:
Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang (Pouzolzia zeylanica (L.) Benn.var.microphylla (Wedd.) W.T.Wang) is the herb of Urticaceae Herba Pouzolziae Zeylanicae platymiscium Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang, have another name called stone strain, Shi Zhuzi, the domestic southeastern Yunnan that is distributed in, Guangxi, Guangdong, Fujian, south, Jiangxi, ground such as Taiwan are widely distributed in the torrid areas, Asia abroad.The nature and flavor hardship, cold, go into lung meridian.Effect with detoxicating, relieving inflammation is used for the treatment of the scorching swollen disease of waiting of furuncle.Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang mainly contains materials such as flavonoid, alkaloids and saponins.
At present, the relevant report of Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang chemical constituent is rarely found, and especially the report of Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang flavone extract is not seen as yet.Therefore, the preparation method that a kind of Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang total flavones is provided is used the Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang flavone for the chemical constituent of further research Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang and clinical development and is significant.
Summary of the invention:
The preparation method that the purpose of this invention is to provide a kind of Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang total flavones.
The present invention is achieved by the following technical solutions:
A kind of preparation method of Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang total flavones, it is characterized in that may further comprise the steps: be raw material with the Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang, with boiling range is after 60-90 ℃ petroleum ether heat is carried, reuse 50-70% alcoholic solution extracts 2-3 time, extracting solution is condensed into extractum, in extractum, add sour water, leach insoluble matter, the an amount of dissolve with ethanol solution of insoluble matter, add an amount of macroporous resin and stir, volatilize solvent, water and alcoholic solution eluting, the eluent of Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang total flavones is rich in collection, and concentrate drying promptly gets product.
Described extracting method can be selected microwave extracting, ultrasonic extraction or reflux, extract, for use, and extracting temperature is 55-90 ℃, and extraction time is 1-2h.
Described sour water is pH2～4 hydrochloric acid or aqueous sulfuric acid.
A kind of among the optional AB-8 of described macroporous resin model, LSA-21 and the HZ806, the eluting alcoholic solution is the 60-85% alcoholic solution.
The present invention adopts the hot lifting manipulation of petroleum ether to remove oil-soluble impurities, and sour water dissolving effectively removed impurity, has alleviated resin absorption is disturbed, and resin is strengthened the flavone absorbability, and cost is low, and technology is reasonable, the purity height.
Further specify the present invention below in conjunction with the specific embodiment, but the scope of protection of present invention is not limited to following embodiment.
The specific embodiment:
Embodiment 1:
Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang is pulverized, get 1kg, after carrying 1h with petroleum ether (boiling range is 60-90 ℃) heat, reuse 50% alcoholic solution microwave extracting 2 times, extracting temperature is 90 ℃, each 1h, extracting solution is condensed into extractum, in extractum, add the pH2 aqueous hydrochloric acid solution, leach insoluble matter, an amount of dissolve with ethanol solution of insoluble matter, adding 500g HZ806 macroporous resin stirs, volatilize solvent, the dress post, it is colourless to be washed till lower column liquid with distilled water earlier, reuse 75% alcoholic solution eluting, the eluent of Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang total flavones is rich in collection, and concentrate drying promptly gets product 7.8g, and content is 65.2%.
Embodiment 2:
Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang is pulverized, get 1kg, after carrying 1h with petroleum ether (boiling range is 60-90 ℃) heat, reuse 70% alcoholic solution reflux, extract, 3 times, extracting temperature is 80 ℃, each 2h, extracting solution is condensed into extractum, in extractum, add the pH4 aqueous hydrochloric acid solution, leach insoluble matter, an amount of dissolve with ethanol solution of insoluble matter, adding 500g AB-8 macroporous resin stirs, volatilize solvent, the dress post, it is colourless to be washed till lower column liquid with distilled water earlier, reuse 75% alcoholic solution eluting, the eluent of Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang total flavones is rich in collection, and concentrate drying promptly gets product 14.5g, and content is 65.8%.
Embodiment 3:
Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang is pulverized, get 1kg, after carrying 1h with petroleum ether (boiling range is 60-90 ℃) heat, reuse 60% alcoholic solution microwave extracting 2 times, extracting temperature is 55 ℃, each 2h, extracting solution is condensed into extractum, in extractum, add the pH3 aqueous sulfuric acid, leach insoluble matter, an amount of dissolve with ethanol solution of insoluble matter, adding 500g LSA-21 macroporous resin stirs, volatilize solvent, the dress post, it is colourless to be washed till lower column liquid with distilled water earlier, reuse 80% alcoholic solution eluting, the eluent of Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang total flavones is rich in collection, and concentrate drying promptly gets product 7.7g, and content is 78.6%.
Embodiment 4:
Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang is pulverized, get 1kg, after carrying 1h with petroleum ether (boiling range is 60-90 ℃) heat, reuse 70% alcoholic solution reflux, extract, 2 times, extracting temperature is 85 ℃, each 1h, extracting solution is condensed into extractum, in extractum, add the pH2 aqueous sulfuric acid, leach insoluble matter, an amount of dissolve with ethanol solution of insoluble matter, adding the 800gLSA-21 macroporous resin stirs, volatilize solvent, the dress post, it is colourless to be washed till lower column liquid with distilled water earlier, reuse 85% alcoholic solution eluting, the eluent of Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang total flavones is rich in collection, and concentrate drying promptly gets product 6.7g, and content is 85.0%.
Embodiment 5:
Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang is pulverized, get 1kg, after carrying 1h with petroleum ether (boiling range is 60-90 ℃) heat, reuse 70% alcoholic solution ultrasonic extraction 3 times, extracting temperature is 55 ℃, each 1h, extracting solution is condensed into extractum, in extractum, add the pH2 aqueous hydrochloric acid solution, leach insoluble matter, an amount of dissolve with ethanol solution of insoluble matter, adding 800g AB-8 macroporous resin stirs, volatilize solvent, the dress post, it is colourless to be washed till lower column liquid with distilled water earlier, reuse 60% alcoholic solution eluting, the eluent of Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang total flavones is rich in collection, and concentrate drying promptly gets product 8.2g, and content is 75.0%.
Claims (4)
1. the preparation method of a Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang total flavones, it is characterized in that may further comprise the steps: be raw material with the Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang, with boiling range is after 60-90 ℃ petroleum ether heat is carried, reuse 50-70% alcoholic solution extracts 2-3 time, extracting solution is condensed into extractum, in extractum, add sour water, leach insoluble matter, the an amount of dissolve with ethanol solution of insoluble matter, add an amount of macroporous resin and stir, volatilize solvent, water and alcoholic solution eluting, the eluent of Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang total flavones is rich in collection, and concentrate drying promptly gets product.
2. the preparation method of a kind of Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang total flavones according to claim 1 is characterized in that described extracting method can select microwave extracting, ultrasonic extraction or reflux, extract, for use, and extracting temperature is 55-90 ℃, and extraction time is 1-2h.
3. the preparation method of a kind of Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang total flavones according to claim 1 is characterized in that described sour water is pH2～4 hydrochloric acid or aqueous sulfuric acid.
4. the preparation method of a kind of Pouzolzia zeylanica (L.) Benn. Var. Micro-nhylla (Wedd) W. T. Wang total flavones according to claim 1 is characterized in that a kind of among the optional AB-8 of described macroporous resin model, LSA-21 and the HZ806, and the eluting alcoholic solution is the 60-85% alcoholic solution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103333176A (en) * | 2013-06-18 | 2013-10-02 | 广东药学院 | Norlignan compounds and method of separating and verifying norlignan compounds from pouzolzia zeylanica var. microphylla |
| CN105954450A (en) * | 2016-03-23 | 2016-09-21 | 广东药学院 | HPLC fingerprint spectrum of pouzolzia zeylanica var. microphylla medicinal material or general flavonoids of pouzolzia zeylanica var. microphylla and building method and application of HPLC fingerprint spectrum |
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2011
- 2011-05-06 CN CN2011101179195A patent/CN102228486A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103333176A (en) * | 2013-06-18 | 2013-10-02 | 广东药学院 | Norlignan compounds and method of separating and verifying norlignan compounds from pouzolzia zeylanica var. microphylla |
| CN103333176B (en) * | 2013-06-18 | 2015-04-15 | 广东药学院 | Norlignan compounds and method of separating and verifying norlignan compounds from pouzolzia zeylanica var. microphylla |
| CN105954450A (en) * | 2016-03-23 | 2016-09-21 | 广东药学院 | HPLC fingerprint spectrum of pouzolzia zeylanica var. microphylla medicinal material or general flavonoids of pouzolzia zeylanica var. microphylla and building method and application of HPLC fingerprint spectrum |
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Application publication date: 20111102 |