CN100586449C - Method for preparing white peony root total glycosides extract - Google Patents
Method for preparing white peony root total glycosides extract Download PDFInfo
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- CN100586449C CN100586449C CN200810106912A CN200810106912A CN100586449C CN 100586449 C CN100586449 C CN 100586449C CN 200810106912 A CN200810106912 A CN 200810106912A CN 200810106912 A CN200810106912 A CN 200810106912A CN 100586449 C CN100586449 C CN 100586449C
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- paeoniae alba
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Abstract
The invention provides a new method for preparing total glucosides of paeony extract, comprising crude extraction, dissolution, purification and such steps, crude extract is extracted by using a hydrophilic solvent, the purification adopts a macroporous absorption resin to carry out absorption and separation; the method of the invention can greatly improve the content of paeoniflorin to 60 percentto 90 percent, the method has simple operation and lower cost, and the resin can be repeatedly used, which is applicable to industrial production.
Description
Technical field:
The invention relates to a kind of technology of from Chinese crude drug, extracting the high-load Chinese medicinal ingredients, relate to extract in the medicine Radix Paeoniae Alba therefrom the production technology of active ingredient Radix Paeoniae Alba total glucosides specifically.
Background technology:
The Chinese medicine Radix Paeoniae Alba is the dry root of ranunculaceae plant Radix Paeoniae, has the suppressing the hyperactive liver pain relieving, nourishing blood for regulating menstruation, astringing YIN to stop sweating effect; It is dizzy to be used to have a headache, hypochondriac pain, stomachache, limb pain twin, blood deficiency and yellow complexion, menoxenia, spontaneous perspiration, night sweat.Pharmacological research shows that the Radix Paeoniae Alba has effects such as spasmolysis and analgesia, immunomodulating, antiinflammatory.The main effective ingredient that contains in the Radix Paeoniae Alba is peoniflorin, lactone glucoside of Radix Paeoniae, oxypaeoniflorin, benzoylpaeoniflorin etc., is collectively referred to as Radix Paeoniae Alba total glucosides, and wherein paeoniflorin content is more, is one of its main effective ingredient.
The CN88104779 Chinese patent discloses a kind of extracting method, and this method adopts alcohol reflux, ethyl acetate extraction, the technology of concentrate drying.The CN97101960 Chinese patent discloses a kind of new method, and this method adopts alcohol-aqueous solvent reflux, extract,, with alcohol-ester solution extraction, the technology of concentrate drying.Content of paeoniflorin generally can only reach 30%～50% in the Radix Paeoniae Alba extract that these two kinds of technologies are extracted, and content is lower, not too is fit to the pharmacy needs; China Patent No. ZL00121532 discloses and has used aluminium sesquioxide column chromatography purification Radix Paeoniae Alba total glucosides in a kind of preparation injection process, make its paeoniflorin content can reach 80%, but the not reproducible use of aluminium sesquioxide in the aluminium sesquioxide column chromatography, be not suitable for the requirement of industrialized great production, its cost is also high.
Summary of the invention:
Purpose of the present invention just provides a kind of method for preparing the Radix Paeoniae Alba total glucosides extract.
Concrete technology of the present invention is as follows:
1, slightly carries: white Peony Root, decoction pieces or coarse powder raw material, adopt 20%～90% hydrophilic water solution of 5～15 times of Radix Paeoniae Alba dry weights (W/W), under 50～95 degrees celsius, extract 1～3 time, each 1～3 hour, merge extractive liquid, filters, and filtrate is through decompression and solvent recovery, vacuum concentration or be spray dried to Radix Paeoniae Alba crude extract, described hydrophilic water solution is one or several mixed solvents in methanol, ethanol, propanol, isopropyl alcohol, the acetone.
2, dissolving: Radix Paeoniae Alba crude extract is made aqueous solution or little suspendible shape solution with hydrophilic solvent dissolving and filtration, and adjusting pH value with diluted alkaline is 4～9.
Described hydrophilic solvent is one or several mixed solvents in methanol, ethanol, propanol, isopropyl alcohol, the acetone; Used alkali is: NaHCO
3, NaOH, KHCO
3, a kind of among the KOH, the consumption of described hydrophilic solvent is 1～50 times of Radix Paeoniae Alba crude extract weight.
3, purification adopts macroporous adsorbent resin that aqueous solution is adsorbed, be adsorbed to saturated after, wash decontamination earlier with water to the Molish reaction negative, 1～10 times of amount of resin of the hydrophilic solvent of 20%～90% final concentration of 2～20 times of amount of resin of reuse/hour flow velocity (V/H) eluting target substance, eluent decompression backwater solvent, vacuum drying or spray drying are made the Radix Paeoniae Alba total glucosides extract.
Described macroporous adsorbent resin is HPD-100, HPD-300, HPD-400, HPD-500, HPD-600, the HPD-700 of polystyrene skeleton, among the HPD-800 one or more; Or among the D101 of polyacrylic acid skeleton, DK110, the DK113 one or more.
Macroporous adsorbent resin is a kind of polymer absorbant with porous three dimensional structure synthetic, it is a class new type resin that on ion-exchanger and other adsorbent application foundation, grows up, be the Van der Waals force that relies between it and the molecule (adsorbate) that is adsorbed, undertaken by its huge specific surface that physical absorption works.In actual applications to some molecules close such as the very strong absorbability of the outstanding tool of aromatic series ring-type chemical compound with its framing structure.The present invention has improved content of paeoniflorin greatly owing to adopted the macroporous resin adsorption isolation technics, reaches 60%～90%, and this technological operation is easy, and cost is lower, and resin can use repeatedly, is fit to commercial production.
The used content assaying method of the present invention is the high effective liquid chromatography for measuring paeoniflorin content: chromatographic condition is for being filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.1% phosphoric acid solution (14: 86) is mobile phase; The detection wavelength is 230nm; Reference substance is a peoniflorin.Number of theoretical plate calculates by the peoniflorin peak should be not less than 2000
Embodiment 1
100G Radix Paeoniae Alba decoction pieces is put into the hydrophilic water solution methanol of 5 times of its weight, under 50 degrees celsius, extract 1～3 time, each 2 hours, merge extractive liquid,, filter, filtrate is through decompression and solvent recovery, vacuum concentration or be spray dried to Radix Paeoniae Alba crude extract, the hydrophilic solvent ethanol of gained Radix Paeoniae Alba crude extract being put into 10 times of its weight dissolves, and uses diluted alkaline NaHCO
3Adjusting pH value is 4, adopt the HPD-100 macroporous adsorbent resin of polystyrene skeleton that aqueous solution is adsorbed, be adsorbed to saturated after, wash decontamination earlier with water to the Molish reaction negative, 3 times of amount of resin of the hydrophilic solvent of 20%～90% final concentration of 5 times of amount of resin of reuse/hour flow velocity (V/H) eluting target substance, eluent decompression backwater solvent, vacuum drying or spray drying are made the Radix Paeoniae Alba total glucosides extract.
Embodiment 2
100G Radix Paeoniae Alba decoction pieces is put into the hydrophilic water solution ethanol of 10 times of its weight, under 70 degrees celsius, extract 1～3 time, each 3 hours, merge extractive liquid,, filter, filtrate is through decompression and solvent recovery, vacuum concentration or be spray dried to Radix Paeoniae Alba crude extract, the hydrophilic solvent ethanol of gained Radix Paeoniae Alba crude extract being put into 20 times of its weight dissolves, adjusting pH value with diluted alkaline NaOH is 6, adopt the HPD-300 macroporous adsorbent resin of polystyrene skeleton that aqueous solution is adsorbed, be adsorbed to saturated after, wash decontamination earlier with water to the Molish reaction negative, 3 times of amount of resin of the hydrophilic solvent of 20%～90% final concentration of 10 times of amount of resin of reuse/hour flow velocity (V/H) eluting target substance, eluent decompression backwater solvent, vacuum drying or spray drying are made the Radix Paeoniae Alba total glucosides extract.
Embodiment 3
100G Radix Paeoniae Alba decoction pieces is put into the hydrophilic water solution propanol of 15 times of its weight, under 95 degrees celsius, extract 1～3 time, each 1 hour, merge extractive liquid,, filter, filtrate is through decompression and solvent recovery, vacuum concentration or be spray dried to Radix Paeoniae Alba crude extract, the hydrophilic solvent ethanol of gained Radix Paeoniae Alba crude extract being put into 40 times of its weight dissolves, adjusting pH value with diluted alkaline KHCO3 is 9, adopt the D101 macroporous adsorbent resin of polyacrylic acid skeleton that aqueous solution is adsorbed, be adsorbed to saturated after, wash decontamination earlier with water to the Molish reaction negative, 10 times of amount of resin of the hydrophilic solvent of 20%～90% final concentration of 20 times of amount of resin of reuse/hour flow velocity (V/H) eluting target substance, eluent decompression backwater solvent, vacuum drying or spray drying are made the Radix Paeoniae Alba total glucosides extract.
Claims (1)
1, a kind of method for preparing the Radix Paeoniae Alba total glucosides extract, its concrete technology is as follows:
1), slightly carries: white Peony Root, decoction pieces or coarse powder raw material, adopt 20%～90% hydrophilic water solution of 5～15 times of Radix Paeoniae Alba dry weights (W/W), under 50～95 degrees celsius, extract 1～3 time, each 1～3 hour, merge extractive liquid, filters, and filtrate is through decompression and solvent recovery, vacuum concentration or be spray dried to Radix Paeoniae Alba crude extract, described hydrophilic water solution is one or several mixed solvents in methanol, ethanol, propanol, isopropyl alcohol, the acetone;
2), dissolving: Radix Paeoniae Alba crude extract is made aqueous solution or little suspendible shape solution with hydrophilic solvent dissolving and filtration, and adjusting pH value with diluted alkaline is 4～9;
Described hydrophilic solvent is one or several mixed solvents in methanol, ethanol, propanol, isopropyl alcohol, the acetone; Used alkali is: NaHCO
3, NaOH, KHCO
3, a kind of among the KOH, the consumption of described hydrophilic solvent is 1～50 times of Radix Paeoniae Alba crude extract weight;
3) purification adopts macroporous adsorbent resin that aqueous solution is adsorbed, be adsorbed to saturated after, wash decontamination earlier with water to the Molish reaction negative, 1～10 times of amount of resin of the hydrophilic solvent of 20%～90% final concentration of 2～20 times of amount of resin of reuse/hour flow velocity (V/H) eluting target substance, eluent decompression backwater solvent, vacuum drying or spray drying are made the Radix Paeoniae Alba total glucosides extract;
Described macroporous adsorbent resin is HPD-100, HPD-300, HPD-400, HPD-500, HPD-600, the HPD-700 of polystyrene skeleton, among the HPD-800 one or more; Or among the D101 of polyacrylic acid skeleton, DK110, the DK113 one or more.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200810106912A CN100586449C (en) | 2008-06-13 | 2008-06-13 | Method for preparing white peony root total glycosides extract |
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| CN200810106912A CN100586449C (en) | 2008-06-13 | 2008-06-13 | Method for preparing white peony root total glycosides extract |
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| CN100586449C true CN100586449C (en) | 2010-02-03 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101607975B (en) * | 2009-07-16 | 2011-07-20 | 宁波立华植物提取技术有限公司 | Method for separating and preparing peony lactone glucoside by simulation moving bed chromatography method |
| CN102824423B (en) * | 2012-09-18 | 2014-01-15 | 宁波立华制药有限公司 | Medicinal composition comprising albiflorin and arctiin and application |
| CN107271601B (en) * | 2017-01-19 | 2019-06-11 | 安徽九洲方圆制药有限公司 | A kind of discrimination method of Radix-paeoniae-rubra formula granules and white peony root dispensing granule |
| CN108079072A (en) * | 2017-12-12 | 2018-05-29 | 浙江中医药大学 | A kind of preparation method for treating the total glucoside of allergic asthma and its application in allergic asthma treatment |
| 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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2008
- 2008-06-13 CN CN200810106912A patent/CN100586449C/en active Active
Non-Patent Citations (4)
| Title |
|---|
| HPD100大孔吸附树脂在白芍纯化工艺中的应用研究. 张亚军，徐莲英.中药材，第29卷第9期. 2006 |
| HPD100大孔吸附树脂在白芍纯化工艺中的应用研究. 张亚军，徐莲英.中药材，第29卷第9期. 2006 * |
| 正交试验法优选白芍中芍药苷的提取工艺研究. 吴悟贤，李生才，牛之猛.时珍国医国药，第14卷第7期. 2003 |
| 正交试验法优选白芍中芍药苷的提取工艺研究. 吴悟贤，李生才，牛之猛.时珍国医国药，第14卷第7期. 2003 * |
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