CN1490320A - Preparation of paris polyphylla saponin - Google Patents
Preparation of paris polyphylla saponin Download PDFInfo
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- CN1490320A CN1490320A CNA031355897A CN03135589A CN1490320A CN 1490320 A CN1490320 A CN 1490320A CN A031355897 A CNA031355897 A CN A031355897A CN 03135589 A CN03135589 A CN 03135589A CN 1490320 A CN1490320 A CN 1490320A
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- rhizoma paridis
- total saponins
- paridis total
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- alcohol
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Abstract
A process for preparing the common saponin of Chinese paris rhizome includes such steps as extracting, separating and purifying, and features that the extracting in alcohol, membrane filtering, resin adsorbing, resin decoloring, decoloring with activated carbon and defatting with acetone are combined. Its advantages are high extracting rate and low cost.
Description
Technical field
The present invention relates to a kind of extraction of middle pharmaceutically active ingredient, more specifically say, the present invention relates to the preparation method of Rhizoma Paridis total saponins.
Background technology
Conclusion is got up, and existing Rhizoma Paridis total saponins has ethanol extraction method, n-butanol extraction method and adsorption resin method.These methods, the product that makes are brown, brown or light brown, and appearance luster is darker; Resistance to water soak is poor, saponin content and extraction yield are lower.These weak points are technical barriers anxious to be solved in the Rhizoma Paridis total saponins preparation.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of preparation method of Rhizoma Paridis total saponins is provided.This method can effectively be improved the color and luster and the water absorbability of product, and can improve saponin content and extraction yield.
Purpose of the present invention is achieved by following technical proposals.
Except as otherwise noted, the percentage ratio that is adopted among the present invention is weight percentage.
The invention provides a kind of preparation method of Rhizoma Paridis total saponins, this method comprises the step of following order:
(1) it is an amount of to get Paris (Paris) plant herb, is crushed to meal, adds weight and be 4～10 times aqueous alcohol, 60 ℃～90 ℃ following refluxing extraction three times; United extraction liquid reclaims pure liquid, and the medicinal extract that must wet is about 15%, and proportion is 1.05～1.15;
(2) getting wet medicinal extract, to add weight be 10～30 times aqueous alcohol dissolving, separates through membrane filtration; The liquid that dams is recycled, and gets Rhizoma Paridis total saponins A;
(3) filtrate is through polymeric adsorbent absorption, and effluent liquid discards, again with after the suitable quantity of water washing, with the desorb of 3～5 times of amount aqueous alcohol;
(4) stripping liquid decolours through decolorizing resin, collects effluent liquid, and recovered alcohol promptly gets Rhizoma Paridis total saponins B again after decolouring, filtration and drying;
(5) described Rhizoma Paridis total saponins A and Rhizoma Paridis total saponins B uniform mixing are required Rhizoma Paridis total saponins.
Beneficial effect:
1. the present invention organically is combined into one alcoholic extraction, membrane filtration, polymeric adsorbent, decolorizing resin and unit operations such as gac combination decolouring, acetone degreasing, successfully solves the deficiencies in the prior art.
2. indexs such as product appearance color and luster, resistance to water soak (wettability test moisture content), saponin content and saponin(e extraction yield compared with prior art the results are shown in table 1.
Table 1.
The result of table 1 shows, the Rhizoma Paridis total saponins product appearance color and luster near-white that adopts the present invention to produce, and resistance to water soak is strong, and active constituent content is high and stable, the extraction yield height, production cost is low.
3. process repeatability and constant product quality test-results are listed in table 2.
Table 2
| Lot number | Appearance luster | Resistance to water soak (moisture content) | Saponin content | The saponin(e extraction yield |
| ????20030425 | Near-white | ????2.5％ | ????51％ | ????84％ |
| ????20030513 | Near-white | ????3.5％ | ????59％ | ????87％ |
| ????20030525 | Near-white | ????2.7％ | ????60％ | ????89％ |
| ????20030609 | Near-white | ????4.2％ | ????53％ | ????82％ |
The result of table 2 shows, determined processing condition repeat scale-up through pilot scale repeatedly, and technology quality index repeatability better can be applicable to suitability for industrialized production.
4. the finger printing to product compares, and its result shows product HPLC finger printing repeatability better, and steady quality is reliable, has good prospect in medicine.
Description of drawings
Fig. 1 is total saponin standard substance HPLC collection of illustrative plates;
Fig. 2 is total saponin 20030425HPLC collection of illustrative plates;
Fig. 3 is total saponin 20030513HPLC collection of illustrative plates;
Fig. 4 is total saponin 20030525HPLC collection of illustrative plates;
Fig. 5 is total saponin 2003609HPLC collection of illustrative plates.
Embodiment
By specific embodiment given below, can further be well understood to the present invention.But they are not limitation of the invention.
Embodiment 1
Get Paris polyphylla plant herb 40Kg, be crushed to meal, add 280 liters of 70% alcohol at every turn, 70 ℃ of thermal backflows are extracted three times, 40 order stainless steel sift net filtrations, and filtrate merges, reclaim under reduced pressure alcohol, the medicinal extract 6.2Kg that must wet, proportion 1.1.Wet medicinal extract is added 62 liters of dissolvings of alcohol of 40%, is the ceramic membrane filter separation of 0.2um with the aperture; Other gets 45 liters of 40% alcohol, divides 3 times to the liquid that the dams washing of dialysing.The last liquid that dams (about 13 liters) 50 liters of dissolvings of alcohol with 95%, add 150 gram gacs again, stirring at normal temperature 8 hours, filter paper filtering, filtrate gets white medicinal extract 1156 grams behind reclaim under reduced pressure alcohol, add 5 liters of acetone thermal backflow degreasings 2 hours again, filter paper filtering, white precipitate, according to 50 ℃ of drying under reduced pressure 8 hours, promptly get Rhizoma Paridis total saponins A 956 grams (containing dioscin 51.8%, pennogenin 7.2%) after the pulverizing, filtrate discards after reclaiming acetone.
Merge ceramic membrane filter filtrate and dialyzate, so that per hour 100 liters flow velocity is through macroporous adsorptive resins bed (60 liters of volumes), effluent liquid discards behind reclaim under reduced pressure alcohol, use 150 liters of deionized water wash again after, 150 liters of alcohol with 90% are with per hour 100 liters flow velocity desorb.Stripping liquid with 50 liters flow velocity per hour through macropore decolorizing resin post bed (100 liters), use 100 liters of washings of alcohol of 90% again, collect effluent liquid, reclaim under reduced pressure alcohol, medicinal extract promptly gets Rhizoma Paridis total saponins B 1112 grams (containing dioscin 25.5%, pennogenin 19.8%) through 50 ℃ of drying under reduced pressure 8 hours after the pulverizing.
Above Rhizoma Paridis total saponins A and Rhizoma Paridis total saponins B uniform mixing are required Rhizoma Paridis total saponins 2068 grams (containing dioscin 37.6%, pennogenin 13.9%).
Embodiment 2
Except adding weight in the raw material meal is 10 times aqueous alcohol, outside 90 ℃ of following thermal backflows, other process is with embodiment 1.
Except adding weight in the raw material meal is 4 times aqueous alcohol, outside 60 ℃ of following thermal backflows, other process is with embodiment 1.
Embodiment 4
Get Paris polyphylla plant herb 80Kg, be crushed to meal, add 560 liters of 70% alcohol at every turn, 70 ℃ of thermal backflows are extracted three times, 40 order stainless steel sift net filtrations, and filtrate merges, reclaim under reduced pressure alcohol, the about 12.5Kg of medicinal extract that must wet, proportion about 1.1.More than wet medicinal extract adds 126 liters of dissolvings of alcohol of 40%, is the ceramic membrane filter separation of 0.2um with the aperture, and other gets 45 liters of 40% alcohol, divides 3 times to the liquid that the dams washing of dialysing.The last liquid that dams (about 13 liters) 50 liters of dissolvings of alcohol with 95%, add 300 gram gacs again, stirring at normal temperature 8 hours, filter paper filtering, filtrate gets white medicinal extract 2318 grams behind reclaim under reduced pressure alcohol, add 10 liters of acetone thermal backflow degreasings 2 hours again, filter paper filtering, white precipitate, through 50 ℃ of drying under reduced pressure 8 hours, promptly get Rhizoma Paridis total saponins A 1920 grams (containing dioscin 53.0%, pennogenin 7.1%) after the pulverizing, filtrate discards after reclaiming acetone.
Merge ceramic membrane filter filtrate and dialyzate, so that per hour 100 liters flow velocity is through macroporous adsorptive resins bed (60 liters of volumes), effluent liquid discards behind reclaim under reduced pressure alcohol, use 150 liters of deionized water wash again after, 150 liters of alcohol with 90% are with per hour 100 liters flow velocity desorb.Stripping liquid with 50 liters flow velocity per hour through macropore decolorizing resin post bed (100 liters), use 100 liters of washings of alcohol of 90% again, collect effluent liquid, reclaim under reduced pressure alcohol, medicinal extract promptly gets Rhizoma Paridis total saponins B 2275 grams (containing dioscin 26.7%, pennogenin 18.9%) through 50 ℃ of drying under reduced pressure 8 hours after the pulverizing.
Above Rhizoma Paridis total saponins A and Rhizoma Paridis total saponins B uniform mixing are required Rhizoma Paridis total saponins 4195 grams (containing dioscin 38.7%, pennogenin 13.5%).
Embodiment 5
In described wet medicinal extract, add weight and be 10 times the aqueous alcohol dissolving, other and process and
Embodiment 4 is identical.
Embodiment 6
Get Paris polyphylla plant herb 120Kg, be crushed to meal, add 840 liters of 70% alcohol at every turn, 70 ℃ of thermal backflows are extracted three times, 40 order stainless steel sift net filtrations, and filtrate merges, reclaim under reduced pressure alcohol, the about 18.7Kg of medicinal extract that must wet, proportion 1.1.Wet medicinal extract adds 184 liters of dissolvings of alcohol of 40%, is that the ceramic membrane filter of 0.2um separates with the aperture, and other gets 45 liters of 40% alcohol, divides 3 times to the liquid that the dams washing of dialysing.
The last liquid that dams (about 13 liters) 50 liters of dissolvings of alcohol with 95%, add 450 gram gacs again, stirring at normal temperature 8 hours, filter paper filtering, filtrate gets white medicinal extract 3478 grams behind reclaim under reduced pressure alcohol, add 15 liters of acetone thermal backflow degreasings 2 hours again, filter paper filtering gets white precipitate, through 50 ℃ of drying under reduced pressure 8 hours, promptly get Rhizoma Paridis total saponins A 2901 grams (containing dioscin 52.5%, pennogenin 7.5%) after the pulverizing, filtrate discards after reclaiming acetone.
Merge ceramic membrane filter filtrate and dialyzate, so that per hour 100 liters flow velocity is through macroporous adsorptive resins bed (60 liters of volumes), effluent liquid discards behind reclaim under reduced pressure alcohol, use 150 liters of deionized water wash again after, 150 liters of alcohol with 90% are with per hour 100 liters flow velocity desorb.Stripping liquid with 50 liters flow velocity per hour through macropore decolorizing resin post bed (100 liters), use 100 liters of washings of alcohol of 90% again, collect effluent liquid, reclaim under reduced pressure alcohol, medicinal extract promptly gets Rhizoma Paridis total saponins B3407 gram (containing dioscin 25.7%, pennogenin 19.3%) through 50 ℃ of drying under reduced pressure 8 hours after the pulverizing.
Above Rhizoma Paridis total saponins A and Rhizoma Paridis total saponins B uniform mixing are required Rhizoma Paridis total saponins 6308 grams (containing dioscin 38.0%, pennogenin 13.9%).
Embodiment 7
In described wet medicinal extract, add weight and be 30 times the aqueous alcohol dissolving, other and process and
Embodiment 6 is identical.
Claims (3)
1. the preparation method of a Rhizoma Paridis total saponins, this method comprises the step of following order:
(1) it is an amount of to get Paris (Paris) plant herb, is crushed to meal, adds weight and be 4～10 times aqueous alcohol, 60 ℃～90 ℃ following refluxing extraction three times; United extraction liquid reclaims pure liquid, and the medicinal extract that must wet is about 15%, and proportion is 1.05～1.15;
(2) getting wet medicinal extract, to add weight be 10～30 times aqueous alcohol dissolving, separates through membrane filtration; The liquid that dams is recycled, and gets Rhizoma Paridis total saponins A;
(3) filtrate is through polymeric adsorbent absorption, and effluent liquid discards, again with after the suitable quantity of water washing, with the desorb of 3～5 times of amount aqueous alcohol;
(4) stripping liquid decolours through decolorizing resin, collects effluent liquid, and recovered alcohol promptly gets Rhizoma Paridis total saponins B again after decolouring, filtration and drying;
(5) described Rhizoma Paridis total saponins A and Rhizoma Paridis total saponins B uniform mixing are required Rhizoma Paridis total saponins.
2. the preparation method of Rhizoma Paridis total saponins according to claim 1 is to adopt ceramic membrane filter to separate in the described membrane filtration separation of step (2) wherein; It is to adopt decolorizing with activated carbon that the described liquid that dams is recycled.
3. the preparation method of Rhizoma Paridis total saponins according to claim 1 is to adopt the macroporous adsorptive resins bed in step (3) or (4) described decolorizing resin decolouring wherein.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031355897A CN1490320A (en) | 2003-08-11 | 2003-08-11 | Preparation of paris polyphylla saponin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031355897A CN1490320A (en) | 2003-08-11 | 2003-08-11 | Preparation of paris polyphylla saponin |
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| CN1490320A true CN1490320A (en) | 2004-04-21 |
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| CNA031355897A Pending CN1490320A (en) | 2003-08-11 | 2003-08-11 | Preparation of paris polyphylla saponin |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101513163B (en) * | 2009-04-03 | 2011-05-18 | 武汉大学 | Method for increasing the contents of steroid saponin in paris polyphylla rhizome by penicillium citrinum elicitor |
| CN103739661A (en) * | 2014-01-22 | 2014-04-23 | 长沙湘资生物科技有限公司 | Method for extracting pennogenin from paris polyphylla |
| CN103755775A (en) * | 2014-01-22 | 2014-04-30 | 长沙湘资生物科技有限公司 | Method for extracting dioscin from rhizome of paris polyphylla |
| CN110776541A (en) * | 2019-11-19 | 2020-02-11 | 云南贝泰妮生物科技集团股份有限公司 | Preparation method and application of quercetin-3-gentiobioside |
-
2003
- 2003-08-11 CN CNA031355897A patent/CN1490320A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101513163B (en) * | 2009-04-03 | 2011-05-18 | 武汉大学 | Method for increasing the contents of steroid saponin in paris polyphylla rhizome by penicillium citrinum elicitor |
| CN103739661A (en) * | 2014-01-22 | 2014-04-23 | 长沙湘资生物科技有限公司 | Method for extracting pennogenin from paris polyphylla |
| CN103755775A (en) * | 2014-01-22 | 2014-04-30 | 长沙湘资生物科技有限公司 | Method for extracting dioscin from rhizome of paris polyphylla |
| CN103755775B (en) * | 2014-01-22 | 2015-05-20 | 长沙湘资生物科技有限公司 | Method for extracting dioscin from rhizome of paris polyphylla |
| CN110776541A (en) * | 2019-11-19 | 2020-02-11 | 云南贝泰妮生物科技集团股份有限公司 | Preparation method and application of quercetin-3-gentiobioside |
| CN110776541B (en) * | 2019-11-19 | 2021-08-13 | 云南贝泰妮生物科技集团股份有限公司 | Preparation method and application of quercetin-3-gentiobioside |
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