CN102443028A - Method for extracting paeoniflorin from radix paeoniae lactiflorae - Google Patents
Method for extracting paeoniflorin from radix paeoniae lactiflorae Download PDFInfo
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- CN102443028A CN102443028A CN2010105001182A CN201010500118A CN102443028A CN 102443028 A CN102443028 A CN 102443028A CN 2010105001182 A CN2010105001182 A CN 2010105001182A CN 201010500118 A CN201010500118 A CN 201010500118A CN 102443028 A CN102443028 A CN 102443028A
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- macroporous resin
- peoniflorin
- ethanol
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- elutriant
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Abstract
The invention relates to a method for extracting paeoniflorin from radix paeoniae lactiflorae. The process method comprises the following steps: crushing medicinal radix paeoniae lactiflorae materials; carrying out ultrasonic extraction with an acidic alcohol or ketone solution; adding polar macroporous resin into the concentrated solution for adsorption; eluting with 40-70% acidic ethanol; recovering ethanol in the eluent; adding nonpolar macroporous resin for adsorption; eluting with 30-50% methanol; allowing the eluent to pass through an acidic aluminum oxide short column; concentrating, adding a mixed solution of ethyl acetate and n-butyl alcohol, and extracting for 3-5 times; and carrying out vacuum drying to obtain the product. The method for producing paeoniflorin has the advantages of high yield and high content, thereby being applicable to industrial preparation.
Description
Technical field:
The present invention relates to a kind of method of from the root of herbaceous peony, extracting peoniflorin, particularly a kind of method of from the root of herbaceous peony, extracting the high-content peoniflorin.
Background technology:
Peoniflorin is the amorphous white powder of water absorbability, is colourless needle crystal in four acetic esters, fusing point: 196 ℃.Paeoniflorin stable (pH2～6) under sour environment, being heated is prone to decompose.
Paeoniflorin has significant analgesia, calmness, anticonvulsant action, also can coronary artery dilator, increase coronary flow, and the antagonism acute myocardial ischemia brings high blood pressure down, and also has simultaneously to protect the liver, and is antitumor, improve the body immunity effect.The clinical treatment that is used for coronary heart disease; Be used for geriatric disease, build up health with aspect, the especially treatments of senile chronic respiratory tract disease such as immunologic function, anti-inflammatory cough-relieving, eliminating phlegm and relieving asthma in can make ancillary drug.
The peoniflorin process for extracting is more:
Patent " preparation method of extract product of paeoniflorin ", this patent disclosed method are to get radix paeoniae rubrathe medicinal material, pulverize aqueous ethanolic solution; Thermal backflow is extracted, and goes up macroporous adsorptive resins again, ethanol elution; Collect ethanol eluate, concentrate the back and go up polyamide column, water elution; Concentrate eluant gets white powder after the drying.
Patent " extract of total glucosides of paeony and preparation method thereof "; This patent disclosed method is can be by any one methods such as solvent-extraction process, macroporous adsorbent resin method, supercritical fluid extraction, column chromatography, liquid-liquid counter partition chromatographies, or the arbitrary combination of these methods prepares peoniflorin.
Patent " a kind of extraction process of high-content effective composition from white peony root ", this patent disclosed method alcohol-water solution is extracted, and uses the alcohol ester solution extraction, through concentrate drying, gets root of herbaceous peony crude extract, carries out fractionation by adsorption with macroporous adsorbent resin again.
Patent " extraction process of paeoniflorin ", this patent disclosed method are to extract: with raw material section or coarse grain, and the adding enzyme carries out enzymolysis; Add suitable quantity of water and decoct, last macroporous adsorptive resins is used ethanol elution again; Add activated carbon decolorizing after elutriant is heated and filter, use the ETHYLE ACETATE crystallization again.
Document " research of peoniflorin in the high speed adverse current chromatogram separation and purification root of herbaceous peony ", the document adopts microwave extraction, and adverse current chromatogram prepares peoniflorin.
But existing technology exists yield low at preparation high-content peoniflorin, the problem that preparation amount is little, or the problem of technology poor reproducibility.
Summary of the invention:
The technical problem that the present invention will solve provides a kind of method of from the root of herbaceous peony, extracting peoniflorin, and this method can access the high-content product, and is easy to industriallization.
The objective of the invention is to realize like this:
A kind of method of from the root of herbaceous peony, extracting peoniflorin is characterized in that comprising following step:
Extract: the root of herbaceous peony is pulverized, add that 5-15 doubly measures acid alcohol or ketone solution extracts supersound extraction 1-3 time, regulate neutral the filtration, reclaim under reduced pressure reagent gets liquid concentrator;
Macroporous resin adsorption: above-mentioned liquid concentrator is added macroporous resin adsorption, and washing to sugared reaction negative is doubly measured 40-70% acidic ethanol wash-out with 5-8; Elutriant is transferred the neutral ethanol that reclaims; Add the absorption of macroporous resin adsorption post again, 5-7 doubly measures the 30-50% methanol-eluted fractions, collects elutriant;
The alumina column removal of impurities: above-mentioned elutriant adds alumina, collects lower column liquid;
Extraction: above-mentioned lower column liquid reduces pressure back ethanol to small volume, adds ETHYLE ACETATE propyl carbinol mixing solutions extraction 3-5 time, collects organic phase, and drying under reduced pressure promptly gets product.
Alcohol in the said step 1) is ethanol or the methanol solution of 60-80%, and ketone is the acetone soln of 40-70%, and hydrochloric acid or sulfuric acid are regulated pH1-3, ultrasonic power 2～25kw.
Said step 2) macroporous resin column in is: first macroporous resin column is polar macroporous resin column, a kind of among optional NKA-9, NKA-2, LSA-21 and the HZ806; For the second time macroporous resin column is the non-polar macroporous resin post, a kind of among optional X-5, HPD-100 and the D-101.
Aluminum oxide in the said step 3) is an acidic alumina.
ETHYLE ACETATE is 3 with the propyl carbinol ratio in the said step 4): 1-3.
There is following advantage in the present invention: the acid organic reagent supersound extraction time is short, and impurity is few; Polarity and the coupling of non-polar macroporous resin post can make paeoniflorin content reach 85%, and single resin column can't be realized; The acidic alumina short column, it is fast to cross post speed; The extraction of ETHYLE ACETATE propyl carbinol mixing solutions.
Embodiment:
Embodiment 1:
The root of herbaceous peony is pulverized, get 5kg, drop in the supersound extraction jar, dispose 60% ethanolic soln hydrochloric acid and transfer pH value of solution 2; Added 50L supersound extraction (power 2kw) 1 hour, and extracted 2 times, merge extracted twice liquid and regulate neutral filtration, decompression recycling ethanol with sodium hydroxide solution; Get liquid concentrator, add water-dispersion, add 5L NKA-9 macroporous resin adsorption, flow velocity 5kg/h; Absorption finishes, and washes sugared reaction negative, the ethanolic soln wash-out of 25L70%pH3 again, and elutriant is transferred the neutral ethanol that reclaims; Add the absorption of 3LHPD-100 macroporous resin adsorption post again, flow velocity 1.5kg/h, the 18L40% methanol-eluted fractions is collected elutriant; Elutriant adds 2L acidic alumina short column, collects lower column liquid, and the ethanol that reduces pressure back adds 3L ETHYLE ACETATE propyl carbinol (3: 1) mixing solutions to 1L; Concussion is evenly collected organic phase, extracts 3 times, and it is 94.3% peoniflorin finished product that drying under reduced pressure promptly gets 51g content.
Embodiment 2:
The root of herbaceous peony is pulverized, get 5kg, drop in the supersound extraction jar, dispose 70% methanol solution sulfuric acid and transfer pH value of solution 1, added 25L supersound extraction (power 2kw) 0.5 hour; Extract 3 times, merge extracted twice liquid and regulate neutral the filtration with potassium hydroxide solution, decompression recycling ethanol gets liquid concentrator, adds water-dispersion; Add 5L NKA-2 macroporous resin adsorption, flow velocity 5kg/h, absorption finishes, and washes sugared reaction negative, again the ethanol elution of 40L40%pH2; Elutriant is transferred the neutral ethanol that reclaims, and adds the absorption of 4L X-5 macroporous resin adsorption post again, flow velocity 2kg/h, and the 28L methanol-eluted fractions is collected elutriant; Elutriant adds 3L acidic alumina short column, collects lower column liquid, and the ethanol that reduces pressure back adds 2L ETHYLE ACETATE propyl carbinol (3: 2) mixing solutions to 2L; Concussion is evenly collected organic phase, extracts 5 times, and it is 95.3% peoniflorin finished product that drying under reduced pressure promptly gets 62g content.
Embodiment 3:
The root of herbaceous peony is pulverized, get 5kg, drop in the supersound extraction jar, dispose 50% acetone soln hydrochloric acid and transfer pH value of solution 3; Added 40L supersound extraction (power 3kw) 1 hour, and extracted 2 times, merge extracted twice liquid and regulate neutral filtration, decompression recycling ethanol with sodium hydroxide solution; Get liquid concentrator, add water-dispersion, add 5L LSA-21 macroporous resin adsorption, flow velocity 5kg/h; Absorption finishes, and washes sugared reaction negative, the ethanol elution of 30L60%pH1 again, and elutriant is transferred the neutral ethanol that reclaims; Add the absorption of 3L D-101 macroporous resin adsorption post again, flow velocity 2kg/h, 18L40% first wash-out is collected elutriant; Elutriant adds 3L acidic alumina short column, collects lower column liquid, and the ethanol that reduces pressure back adds 2L ETHYLE ACETATE propyl carbinol (1: 1) mixing solutions to 1.5L; Concussion is evenly collected organic phase, extracts 4 times, and it is 95% peoniflorin finished product that drying under reduced pressure promptly gets 56g content.
Embodiment 4:
The root of herbaceous peony is pulverized, get 10kg, drop in the supersound extraction jar, dispose 60% methanol solution hydrochloric acid and transfer pH value of solution 2, add 80L ultrasonic (power 10kw) and extracted 1 hour; Extract 2 times, merge extracted twice liquid and regulate neutral the filtration with sodium hydroxide solution, decompression recycling ethanol gets liquid concentrator, adds water-dispersion; Add 12L HZ806 macroporous resin adsorption, flow velocity 15kg/h washes sugared reaction negative, the ethanol elution of 60L60%pH3 again, and elutriant is transferred the neutral ethanol that reclaims; Add the absorption of 5L HPD-100 macroporous resin adsorption post again, flow velocity 4kg/h, the 35L30% methanol-eluted fractions is collected elutriant; Elutriant adds 5L acidic alumina short column, collects lower column liquid, and the ethanol that reduces pressure back adds 4L ETHYLE ACETATE propyl carbinol (2: 1) mixing solutions to 3L; Stir, collect organic phase, extract 4 times, it is 94.4% peoniflorin finished product that drying under reduced pressure promptly gets 110g content.
Claims (5)
1. method of from the root of herbaceous peony, extracting peoniflorin is characterized in that comprising following step:
1) extract: the root of herbaceous peony is pulverized, add that 5-15 doubly measures acid alcohol or ketone solution extracts supersound extraction 1-3 time, regulate neutral the filtration, reclaim under reduced pressure reagent gets liquid concentrator;
2) macroporous resin adsorption: above-mentioned liquid concentrator is added macroporous resin adsorption, and washing to sugared reaction negative is doubly measured 40-70% acidic ethanol wash-out with 5-8; Elutriant is transferred the neutral ethanol that reclaims; Add the absorption of macroporous resin adsorption post again, 5-7 doubly measures the 30-50% methanol-eluted fractions, collects elutriant;
3) alumina column removal of impurities: above-mentioned elutriant adds alumina, collects lower column liquid;
4) extraction: above-mentioned lower column liquid reduces pressure back ethanol to small volume, adds ETHYLE ACETATE propyl carbinol mixing solutions extraction 3-5 time, collects organic phase, and drying under reduced pressure promptly gets product.
2. according to the preparation method of the said peoniflorin of claim 1, it is characterized in that the alcohol in the said step 1) is ethanol or the methanol solution of 60-80%, ketone is the acetone soln of 40-70%, and hydrochloric acid or sulfuric acid are regulated pH1-3, ultrasonic power 2～25kw.
3. according to the preparation method of the said peoniflorin of claim 1, it is characterized in that said step 2) in macroporous resin column be: first macroporous resin column is polar macroporous resin column, a kind of among the optional NKA-9 of model, NKA-2, LSA-21 and the HZ806; For the second time macroporous resin column is the non-polar macroporous resin post, a kind of among the optional X-5 of model, HPD-100 and the D101.
4. according to the preparation method of the said peoniflorin of claim 1, it is characterized in that the aluminum oxide in the said step 3) is an acidic alumina.
5. according to the preparation method of the said peoniflorin of claim 1, it is characterized in that ETHYLE ACETATE is 3 with the propyl carbinol ratio in the said step 4): 1-3.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010105001182A CN102443028A (en) | 2010-10-09 | 2010-10-09 | Method for extracting paeoniflorin from radix paeoniae lactiflorae |
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| CN2010105001182A CN102443028A (en) | 2010-10-09 | 2010-10-09 | Method for extracting paeoniflorin from radix paeoniae lactiflorae |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103059080A (en) * | 2012-12-13 | 2013-04-24 | 大兴安岭林格贝有机食品有限责任公司 | Process for separating and purifying paeoniflorin |
| CN103792307A (en) * | 2012-10-26 | 2014-05-14 | 中国石油化工股份有限公司 | Extraction liquid for testing of phthalic acid ester content in polyvinyl chloride (PVC) product and its applications |
| CN105726476A (en) * | 2016-04-28 | 2016-07-06 | 河南泰丰生物科技有限公司 | Preparation method of Shaobei injection |
| CN110396117A (en) * | 2019-08-27 | 2019-11-01 | 山东花物堂生物科技有限公司 | The optimal extraction technology of Paeoniflorin and the application in cosmetics in a kind of Radix Paeoniae Alba |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2317613A (en) * | 1996-09-28 | 1998-04-01 | Essential Nutrition Ltd | A method for producing an extract from paeonia containing high levels of paeoniflorin |
| US20020038020A1 (en) * | 2000-09-25 | 2002-03-28 | I-Horng Pan | Process for extracting glycoside using an aqueous two-phase system |
| CN1726965A (en) * | 2005-07-27 | 2006-02-01 | 南京海陵中药制药工艺技术研究有限公司 | Method for preparing extract product of paeoniflorin |
| CN101062128A (en) * | 2007-06-18 | 2007-10-31 | 石任兵 | Extract of total glucosides of paeony and the preparing method thereof |
| WO2009000145A1 (en) * | 2007-06-25 | 2008-12-31 | Zuoguang Zhang | Use and preparation of paeoniflorin and the composition thereof |
-
2010
- 2010-10-09 CN CN2010105001182A patent/CN102443028A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2317613A (en) * | 1996-09-28 | 1998-04-01 | Essential Nutrition Ltd | A method for producing an extract from paeonia containing high levels of paeoniflorin |
| US20020038020A1 (en) * | 2000-09-25 | 2002-03-28 | I-Horng Pan | Process for extracting glycoside using an aqueous two-phase system |
| CN1726965A (en) * | 2005-07-27 | 2006-02-01 | 南京海陵中药制药工艺技术研究有限公司 | Method for preparing extract product of paeoniflorin |
| CN101062128A (en) * | 2007-06-18 | 2007-10-31 | 石任兵 | Extract of total glucosides of paeony and the preparing method thereof |
| WO2009000145A1 (en) * | 2007-06-25 | 2008-12-31 | Zuoguang Zhang | Use and preparation of paeoniflorin and the composition thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103792307A (en) * | 2012-10-26 | 2014-05-14 | 中国石油化工股份有限公司 | Extraction liquid for testing of phthalic acid ester content in polyvinyl chloride (PVC) product and its applications |
| CN103059080A (en) * | 2012-12-13 | 2013-04-24 | 大兴安岭林格贝有机食品有限责任公司 | Process for separating and purifying paeoniflorin |
| CN103059080B (en) * | 2012-12-13 | 2016-01-20 | 大兴安岭林格贝寒带生物科技股份有限公司 | A kind of separation purifying technique of peoniflorin |
| CN105726476A (en) * | 2016-04-28 | 2016-07-06 | 河南泰丰生物科技有限公司 | Preparation method of Shaobei injection |
| CN105726476B (en) * | 2016-04-28 | 2018-06-19 | 河南泰丰生物科技有限公司 | A kind of preparation method of shaobei injection |
| CN110396117A (en) * | 2019-08-27 | 2019-11-01 | 山东花物堂生物科技有限公司 | The optimal extraction technology of Paeoniflorin and the application in cosmetics in a kind of Radix Paeoniae Alba |
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Application publication date: 20120509 |