CN102429965A - Preparation method of active ingredients in cortex moutan - Google Patents
Preparation method of active ingredients in cortex moutan Download PDFInfo
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- CN102429965A CN102429965A CN201110399794XA CN201110399794A CN102429965A CN 102429965 A CN102429965 A CN 102429965A CN 201110399794X A CN201110399794X A CN 201110399794XA CN 201110399794 A CN201110399794 A CN 201110399794A CN 102429965 A CN102429965 A CN 102429965A
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- 239000004480 active ingredient Substances 0.000 title abstract 2
- 238000002360 preparation method Methods 0.000 title abstract 2
- UILPJVPSNHJFIK-UHFFFAOYSA-N Paeonol Chemical compound COC1=CC=C(C(C)=O)C(O)=C1 UILPJVPSNHJFIK-UHFFFAOYSA-N 0.000 claims abstract description 44
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- AVIUTYMRHHBXPB-UXXRCYHCSA-N Paeonoside Natural products COC1=CC=C(C(C)=O)C(O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)=C1 AVIUTYMRHHBXPB-UXXRCYHCSA-N 0.000 description 1
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- XFFQVRFGLSBFON-DEFKTLOSSA-N kaempferol 3,7-di-O-beta-D-glucoside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC(O)=C2C(=O)C(O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O3)O)=C(C=3C=CC(O)=CC=3)OC2=C1 XFFQVRFGLSBFON-DEFKTLOSSA-N 0.000 description 1
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Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a preparation method of each active ingredient in cortex moutan, which is characterized in that cortex moutan raw medicine is percolated in water with the temperature of 25-45 ℃ by 4-6 times in volume to obtain solid-phase dregs and liquid-phase water extract; soaking solid phase in water at room temperature, extracting paeonol by steam distillation, separating liquid phase water extract by gel filtration chromatography to obtain high molecular weight component and low molecular weight component, respectively, extracting cortex moutan polysaccharide from high molecular weight component by alcohol precipitation, and extracting cortex moutan total glycoside from low molecular weight component by macroporous resin adsorption separation. The method comprehensively extracts paeonol, cortex moutan polysaccharide and total paeoniflorin from the cortex moutan, the purity of the obtained cortex moutan polysaccharide is higher than 80%, the purity of the obtained total paeoniflorin is higher than 80%, and the purity of the purified paeonol is higher than 95%.
Description
Technical field
The present invention relates to natural medicine field, the method for preparing of each active component in particularly a kind of Cortex Moutan.
Background technology
The Chinese medicine Cortex Moutan is the dry root bark of ranunculaceae peony (Paeonia suffruticosa Andr.), its cold nature, and acrid in the mouth, hardship, the heart, liver, kidney channel are gone in cold, have heat clearing away, removing heat from blood, and blood, the effect that disappears and become silted up.Paeonol (claiming paeonol again), Cortex Moutan polysaccharide and Cortex Moutan total glycosides (mainly comprising: peoniflorin, benzoylpaeoniflorin, paeonoside, the former glycosides of Cortex Moutan, the new glycosides of Cortex Moutan etc.) are the effective active compositions in the Cortex Moutan; Paeonol has many-sided pharmacological actions such as blood circulation promoting and blood stasis dispelling, clearing away heat and cooling blood, antiinflammatory convergence, analgesia spasmolytic; In medicine, daily use chemicals, field of perfumery purposes is widely arranged; For example make cream and be coated with outward, acute eczema, seborrheic dermatitis, contact dermatitis are had obvious curative effects, be added into and play anti-inflammation and sterilization, the effect hypersensitive of anti-gingiva in the toothpaste; Can also eliminate face acne; To mosquito bite, dermatitis aestivale, miliaria, scalp itch, has antibacterial, a miliaria of dispelling, itching relieving effect, in addition; It waits and to have many-sided pharmacological action the cardiovascular system central nervous system that unifies, and can be used for developing the medicine of anti-cardiovascular system diseases; The Cortex Moutan polysaccharide has higher hypoglycemic activity, can be used for exploitation treatment diabetes medicament, has the important clinical more practical value, also has enhancing human body immunity function and antiinflammatory action etc., effective and safe, no pharmacology toxicity; The Cortex Moutan total glycosides has removes the protective effect of oxygen-derived free radicals regulating liver-QI preferably, can be used for treating hepatitis, its immunomodulating and antiinflammatory action, and the new drug that becomes the treatment rheumatoid arthritis for its exploitation provides possibility.
At present, be confined to a certain active component wherein for the Application and Development overwhelming majority of Cortex Moutan, employed technological means is comparatively outmoded loaded down with trivial details; Production efficiency is lower, and energy resource consumption is big, has also wasted the raw material Cortex Moutan; Limited the application on commercial production; And patent, the bibliographical information of comprehensive simultaneously extraction paeonol, Cortex Moutan polysaccharide and three kinds of active substances of Cortex Moutan total glycosides are few from Cortex Moutan, in order to improve yield, often adopt comparatively loaded down with trivial details method; The instrument and equipment that needs certain scale has limited the application in commercial production.Therefore, set up that a kind of succinct convenience, cost are lower, the method that can extract in the Cortex Moutan three kinds of active substances, economical and efficient, energy-conserving and environment-protective simultaneously is to realizing that the modernization of Chinese medicine has realistic meaning.
Summary of the invention
The object of the invention is to provide a kind of low cost, high efficiency, from Cortex Moutan, obtains the method for preparing of paeonol, Cortex Moutan polysaccharide and each active component of Cortex Moutan total glycosides simultaneously to energy-conserving and environment-protective.
The present invention realizes through following technical scheme: comprise the processing of percolation, separation and liquid phase and solid phase, described percolation is after the Cortex Moutan crude drug is pulverized, and with 4-6 times of volume of 25～45 ℃ of water percolation, separates obtaining solid phase medicinal residues and liquid phase water extracting solution then; It is with gel permeation chromatography extracting solution to be separated that described liquid phase is handled; Obtain high molecular weight component and lower-molecular-weight component according to the appearance time difference; In high molecular weight component, add two volumes concentration 50～90wt% ethanol at least; Leave standstill after stirring, precipitate, collecting precipitation, lyophilizing obtains the Cortex Moutan polysaccharide; The lower-molecular-weight component concentrating under reduced pressure, concentrated solution separates with macroporous resin adsorption, first water elution 4～10 column volumes (BV), ethanol elution is collected with ethanol elution 3～10BV of concentration 20～50wt% in the back, obtains the Cortex Moutan total glycosides after vacuum precipitation, the drying; It is that medicinal residues add hydroecium warm macerating bubble at least 3 hours that described solid phase is handled, and the weight ratio of medicinal residues and water is not less than 1: 5, uses 2.0～2.5kg/cm then
3The steam of pressure carries out vapor distillation, and 110～120 ℃ of control still temperature are collected distillate and cooling, separate, and collecting precipitation obtains paeonol.
Described macroporous resin is selected from D201 or No. 3, precious grace or ASD-8 or AB-8 or HP16 type macroporous resin, and preferred model is a D201 type macroporous resin.
Each active component that obtains can be further purified through known method such as recrystallization.Can use 70% alcoholic solution recrystallization such as paeonol, i.e. 85 ℃ of heating in water bath dissolvings, freezing and crystallizing is at least once.
Beneficial effect of the present invention is: (the Cortex Moutan polysaccharide molecular weight is more than 10kDa according to the difference of Cortex Moutan polysaccharide and Cortex Moutan total glycosides molecular weight size; Cortex Moutan total glycosides molecular weight is less than 1000Da); Use gel permeation chromatography from the Chinese medicine Cortex Moutan, to obtain Cortex Moutan polysaccharide and Cortex Moutan total glycosides; Realized maximum utilization, and cost is lower, is fit to industrial applications medical material; Use D201 type macroporous resin in the Cortex Moutan total glycosides purge process, cost is lower, reliable for effect; The present invention has improved the comprehensive method of extracting paeonol, Cortex Moutan polysaccharide and Cortex Moutan total glycosides from the Chinese medicine Cortex Moutan, and reasonable in design, cost is low, easy to operate, yield is high, is fit to suitability for industrialized production, has a extensive future.
The specific embodiment
Below in conjunction with specific embodiment the present invention is done further explain.
Embodiment one
Get Cortex Moutan crude drug 100g, clean oven dry and pulverize, in the percolation post of packing into, column volume 90ml, with 35 ℃ of warm water of 360mL, flow velocity 200ml/h, percolation separates obtaining medicinal residues and extracting solution; Extracting solution uses Superdex G50 gel permeation chromatography to separate, and obtains containing the macromolecular components and the small molecule component that contains the Cortex Moutan total glycosides of Cortex Moutan polysaccharide; Macromolecular components used 3 times of volume 70% ethanol precipitations 12 hours, and the collecting precipitation lyophilization gets Cortex Moutan polysaccharide part; The small molecule component concentrating under reduced pressure, distillate keeps, macroporous resin column D201 on the concentrated solution (3.5g peoniflorin/kg wet resin); The water flushing 6BV of elder generation remove impurity, reuse 30% ethanol elution 4BV collects eluent and distilling under reduced pressure to there not being the alcohol flavor; Lyophilization promptly gets Cortex Moutan total glycosides part; Medicinal residues added 9.5 times of hydroecium warm macerating bubbles after 5 hours, in alembic, used 2.3kg/cm
3The steam of pressure carries out vapor distillation, 115 ℃ of control still temperature (incorporating the distillate of a step when concentrating permeate into), and heat intermittence; Circulation adds water; End to jar interior original liquid body clarification of discharging and with a small amount of pearl point oil bloom, the collection distillate, the cooling postprecipitation gets the paeonol bullion; Bullion uses 3 times of volume 70% ethanol in 85 ℃ of water-baths, to dissolve, and moves to crystallization in the refrigerator after dissolving fully, and crystallization time is shorter for the first time, to just having crystal to separate out, repeats 3 extremely thoroughly crystallizations of above operation again, gets the pure article of paeonol; Through liquid chromatogram measuring, the yield of Cortex Moutan polysaccharide is 5.0%, and purity is 83%; The yield of Cortex Moutan total glycosides is 6.3%, and purity is (in peoniflorin) 85.3%; The extraction ratio of paeonol is 4.47%, and purity is 99%.
Embodiment two
Get Cortex Moutan crude drug 500g, clean oven dry and pulverize, in the percolation post of packing into, column volume 450ml, with 2700mL35 ℃ of warm water, flow velocity 200ml/h, percolation separates obtaining medicinal residues and extracting solution; Extracting solution uses the Superdex650 gel permeation chromatography to separate, and obtains containing the macromolecular components and the small molecule component that contains the Cortex Moutan total glycosides of Cortex Moutan polysaccharide; Macromolecular components used 3 times of volume 80% ethanol precipitations 12 hours, and the collecting precipitation lyophilization gets Cortex Moutan polysaccharide part; Go up macroporous resin column AB-8 (3.5mg peoniflorin/g wet resin) behind the small molecule component concentrating under reduced pressure; The water flushing 6BV of elder generation remove impurity, reuse 50% ethanol elution 3BV collects eluent and distilling under reduced pressure to there not being the alcohol flavor; Lyophilization promptly gets Cortex Moutan total glycosides part; Medicinal residues added 9.5 times of water logging bubbles after 5 hours, in alembic, used 2.4kg/cm
3The steam of pressure carries out vapor distillation, 115 ℃ of control still temperature (incorporating the distillate of a step when concentrating permeate into), to jar in the original liquid body clarification of discharging and only with a small amount of pearl point oil bloom, the collection distillate cools off postprecipitation and gets the paeonol bullion; Bullion uses 3 times of volume 70% ethanol in 85 ℃ of water-baths, to dissolve, and moves to crystallization in the refrigerator after the dissolving fully, gets the pure article of paeonol; Through liquid chromatogram measuring, the yield of Cortex Moutan polysaccharide is 5.3%, and purity is 86%; The yield of Cortex Moutan total glycosides is 6.6%, and purity (in peoniflorin) is 80.8%, and wherein paeoniflorin content is 41.7%; The extraction ratio of paeonol is 4.16%, and purity is 97%.
Embodiment three
Get Cortex Moutan crude drug 500g, clean oven dry and pulverize, in the percolation post of packing into, column volume 450ml, with 2300mL35 ℃ of warm water, flow velocity 200ml/h, percolation filters medicinal residues and extracting solution; Extracting solution uses Superdex G50 gel permeation chromatography to separate, and obtains containing the macromolecular components and the small molecule component that contains the Cortex Moutan total glycosides of Cortex Moutan polysaccharide; Macromolecular components used 3 times of volume 90% ethanol precipitations 12 hours, and the collecting precipitation lyophilization gets Cortex Moutan polysaccharide part; Go up macroporous resin column D201 (3.5mg peoniflorin/g wet resin) behind the small molecule component concentrating under reduced pressure; The water flushing 6BV of elder generation remove impurity, reuse 50% ethanol elution 3BV collects eluent and distilling under reduced pressure to there not being the alcohol flavor; Lyophilization promptly gets Cortex Moutan total glycosides part; Medicinal residues added 9.5 times of water logging bubbles after 5 hours, in alembic, used 2.3kg/cm
3The steam of pressure carries out vapor distillation, 115 ℃ of control still temperature (incorporating the distillate of a step when concentrating permeate into), to jar in the original liquid body clarification of discharging and only with a small amount of pearl point oil bloom, the collection distillate cools off postprecipitation and gets the paeonol bullion.Bullion uses 3 times of volume 70% ethanol in 85 ℃ of water-baths, to dissolve, and moves to crystallization in the refrigerator after the dissolving fully, gets the pure article of paeonol.Through liquid chromatogram measuring, the yield of Cortex Moutan polysaccharide is 5.0%, and purity is 89%; The yield of Cortex Moutan total glycosides is 6.2%, and purity (in peoniflorin) is 85.8%, and wherein paeoniflorin content is 43.5%; The extraction ratio of paeonol is 4.09%, and purity is 95%.
Claims (6)
1. the method for preparing of each active component in the Cortex Moutan; Comprise the processing of percolation, separation and liquid phase and solid phase; It is characterized in that: described percolation is after the Cortex Moutan crude drug is pulverized, with 4-6 times of volume of 25～45 ℃ of water percolation, to obtain solid phase medicinal residues and liquid phase water extracting solution; It is with gel permeation chromatography extracting solution to be separated that described liquid phase is handled; Obtain high molecular weight component and lower-molecular-weight component according to the appearance time difference; In high molecular weight component, add two volumes concentration 50～90wt% ethanol at least; Leave standstill after stirring, precipitate, collecting precipitation, lyophilizing obtains the Cortex Moutan polysaccharide; The lower-molecular-weight component concentrating under reduced pressure, concentrated solution separates with macroporous resin adsorption, first water elution 4～10BV, ethanol elution is collected with ethanol elution 3～10BV of concentration 20～50wt% in the back, obtains the Cortex Moutan total glycosides after vacuum precipitation, the drying; It is that medicinal residues add hydroecium warm macerating bubble at least 3 hours that described solid phase is handled, and the weight ratio of medicinal residues and water is not less than 1: 5, uses 2.0～2.5kg/cm then
3The steam of pressure carries out vapor distillation, and 110～120 ℃ of control still temperature are collected distillate and cooling, and separation, collecting precipitation obtain paeonol.
2. method for preparing according to claim 1 is characterized in that: after the Cortex Moutan crude drug is pulverized, with 4-6 times of volume of 25～45 ℃ of water percolation.
3. method for preparing according to claim 1 is characterized in that: with gel permeation chromatography extracting solution is separated, obtain high molecular weight component and lower-molecular-weight component according to the appearance time difference.
4. method for preparing according to claim 1 is characterized in that: in high molecular weight component, adds two volumes concentration 50～90wt% ethanol at least, leaves standstill, precipitates after stirring, and collecting precipitation, lyophilizing obtains the Cortex Moutan polysaccharide.
5. method for preparing according to claim 1; It is characterized in that: described macroporous resin is selected from D201 or No. 3, precious grace or ASD-8 or AB-8 or HP16 type macroporous resin; Earlier with water elution 5～8BV; Reuse 30～50wt% ethanol elution 3～5BV collects ethanol elution, obtains the Cortex Moutan total glycosides after vacuum precipitation, the drying.
6. method for preparing according to claim 1 is characterized in that: medicinal residues add hydroecium warm macerating bubble at least 3 hours, and the weight ratio of medicinal residues and water is not less than 1: 5, uses 2.0～2.5kg/cm then
3The steam of pressure carries out vapor distillation, and 110～120 ℃ of control still temperature are collected distillate and cooling, and separation, collecting precipitation obtain paeonol.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103588629A (en) * | 2013-11-18 | 2014-02-19 | 安徽德昌药业饮片有限公司 | Paeonol extraction separation method |
| CN104211589A (en) * | 2014-08-11 | 2014-12-17 | 洛阳莱珂麝薇化妆品有限公司 | Chromatographic separation purification method of paeonol |
| CN117323267A (en) * | 2023-11-20 | 2024-01-02 | 菏泽尧舜牡丹生物科技有限公司 | Peony root bark extract and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103588629A (en) * | 2013-11-18 | 2014-02-19 | 安徽德昌药业饮片有限公司 | Paeonol extraction separation method |
| CN104211589A (en) * | 2014-08-11 | 2014-12-17 | 洛阳莱珂麝薇化妆品有限公司 | Chromatographic separation purification method of paeonol |
| CN117323267A (en) * | 2023-11-20 | 2024-01-02 | 菏泽尧舜牡丹生物科技有限公司 | Peony root bark extract and preparation method thereof |
| CN117323267B (en) * | 2023-11-20 | 2025-11-07 | 菏泽尧舜牡丹生物科技有限公司 | Peony root bark extract and preparation method thereof |
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