CN102250172A - Method for extracting Buddleoside from wild chrysanthemum flowers - Google Patents
Method for extracting Buddleoside from wild chrysanthemum flowers Download PDFInfo
- Publication number
- CN102250172A CN102250172A CN2011101955800A CN201110195580A CN102250172A CN 102250172 A CN102250172 A CN 102250172A CN 2011101955800 A CN2011101955800 A CN 2011101955800A CN 201110195580 A CN201110195580 A CN 201110195580A CN 102250172 A CN102250172 A CN 102250172A
- Authority
- CN
- China
- Prior art keywords
- extracting
- gained
- wild chrysanthemum
- ethyl acetate
- linarin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention discloses a method for extracting Buddleoside from wild chrysanthemum flowers, which comprises the following steps: (1) pretreatment of raw materials; (2) extraction with alkaline water; (3) sedimentation in alcohol; (4) extraction with petroleum ether; (5) acid regulation; (6) separation by macroporous resin absorption; and (7) crystallizing, recrystallizing and drying. The Buddleoside content in the wild chrysanthemum flower extract obtained by the method is up to over 95 percent according to high performance liquid chromatography.
Description
Technical field
The present invention relates to a kind of extracting method of linarin, especially relate to a kind of method of from Wild Chrysanthemum, extracting linarin.
Background technology
Present research about linarin mainly is the research to its pharmacology aspect, and is no matter be domestic or external, comparatively rare to the research report of its extraction process aspect.CN101857621A discloses a kind of method of extracting linarin from Wild Chrysanthemum in 2010.10.13, its typical process flow is to be raw material with the exsiccant Wild Chrysanthemum, through alcohol extracting, concentrate, pH value is regulated, the separation of macroporous resin adsorption wash-out, collect elutriant, again by concentrated, dry, get finished product, finished product linarin content is more than 50%.From three embodiment of its introduction, the preferred embodiment 3 that linarin content is the highest is " more than 60% " (three embodiment all do not provide concrete detection data), infer according to generalized case, and should be below 70%.It is desirable that product purity is still owed.
Summary of the invention
The technical problem to be solved in the present invention is, provides the content of linarin in a kind of product can reach the method for extracting linarin from Wild Chrysanthemum more than 95%.
The technical solution adopted for the present invention to solve the technical problems is: a kind of method of extracting linarin from Wild Chrysanthemum may further comprise the steps:
(1) raw materials pretreatment: with the removal of impurities of exsiccant Wild Chrysanthemum, chopping, use deionized water soak at room temperature 5 ~ 10h, behind the drying water liquid, standby;
(2) potass extraction: adding weight is that the mass concentration of 6 ~ 10 times of Wild Chrysanthemum raw material dry weights is 2 ‰ ~ 8 ‰ alkali aqueous solution, under 70 ℃ ~ 80 ℃ condition, soaks and extracts 〉=2 times, soaks 2 ~ 3h at every turn, filters, and gets extracting solution;
(3) alcohol precipitation: with step (2) gained extracting solution evaporation concentration to former extracting solution heavy 1/20 ~ 1/15, adding weight then is the 95%(volume of 2 ~ 3 times of gained concentrated solutions) ethanol, under 20 ℃ ~ 30 ℃, leave standstill 6 ~ 10h, filter, pure liquid;
(4) extraction: with step (3) gained alcohol liquid evaporation concentration to former gained alcohol liquid measure heavy 1/6 ~ 1/5, add weight then and be the petroleum ether extraction extraction 〉=2 times of 2 ~ 3 times of gained concentrated solutions, collect lower floor's heavy-fluid, upper strata light liquid petroleum ether layer reclaims;
(5) acid adjustment: with step (4) gained heavy-fluid evaporation concentration to its weight 1/3 ~ 1/2 after, to the acid solution that wherein adds 0.2 ~ 0.4 mol/L, regulate pH to 3 ~ 5 after, be cooled to 10 ℃ ~ 20 ℃, leave standstill 10 ~ 20h, the collecting precipitation thing;
(6) macroporous resin adsorption is separated: is 60% ~ 80%(volume with step (5) gained throw out with the concentration that is equivalent to 8 ~ 12 times of weight of precipitate) dissolve with ethanol, last macroporous adsorptive resins, flow velocity is 1.5 ~ 2.0 times of column volume/h, leave standstill 2 ~ 3h, after using 2 ~ 3 times of column volume deionized waters to carry out wash-out, the combination organic solvent that re-uses 8 ~ 12 times of column volumes carries out wash-out, collects the organic solvent elutriant;
(7) crystallization and recrystallization: after step (6) gained had machine eluate evaporation concentration, drying, operating weight is the combination organic solvent dissolution of 10 ~ 15 times of gained dry-matteies, and heat to 40 ℃ ~ 60 ℃, after keeping this temperature 20 ~ 30min, be cooled to 5 ℃ ~ 10 ℃, leave standstill 10 ~ 15h, collect crystal, recrystallization 3 ~ 4 times, the dry finished product that gets.
Further, the preferred sodium hydroxide solution of described 2 ‰ ~ 8 ‰ alkali aqueous solution, sodium carbonate solution or aqua calcis.
Further, the preferred hydrochloric acid of the acid solution of described 0.2 ~ 0.4mol/L, sulfuric acid or phosphoric acid solution.
Further, the preferred D101 of described macroporous adsorbent resin, D1300, HPD450 or AB-8 macroporous adsorbent resin.
Further, used combination organic solvent can be methyl alcohol-ethyl acetate mixed solution during described step (6) wash-out, and wherein methyl alcohol and ethyl acetate weight proportion are 2 ~ 4:1.
Further, used combination organic solvent can be methyl alcohol-ethyl acetate-acetone mixed solution during described step (7) crystallization, and wherein methyl alcohol, ethyl acetate, acetone weight proportion are 1 ~ 2:1 ~ 2:1.
The Flos Chrysanthemi Indici extract product of gained of the present invention detects through high performance liquid chromatography, and its linarin content can reach more than 95%.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1
Present embodiment is realized by following steps:
(1) raw materials pretreatment: with 100 kg exsiccant Wild Chrysanthemum removal of impurities, chopping, use 600kg deionized water soak at room temperature 10h, behind the drying water liquid, standby;
(2) potass extraction: use the sodium hydroxide solution of 1000kg 6 ‰, under 70 ℃ ~ 80 ℃ condition, soak and extract 3 times, soak 2.5h at every turn, filter, get extracting solution;
(3) alcohol precipitation: step (2) gained extracting solution evaporation concentration to 199kg, is added the 95%(volume of 400kg then) ethanol leaves standstill 10h at 20 ℃, filters, and gets pure liquid;
(4) extraction: to 102kg, the petroleum ether extraction of use 300kg 3 times is collected lower floor's heavy-fluid with step (3) gained alcohol liquid evaporation concentration, and upper strata light liquid petroleum ether layer reclaims;
(5) acid adjustment: step (4) gained heavy-fluid evaporation concentration to 34.5kg, to the hydrochloric acid soln that wherein adds 0.2 mol/L, is regulated pH to 3.5, is cooled to 10 ℃, leave standstill 20h after, the collecting precipitation thing;
(6) absorption with macroporous adsorbent resin separates: the dissolve with ethanol 70%(volume that step (5) gained throw out is used 15kg), cross the HPD450 absorption with macroporous adsorbent resin, the control flow velocity is 1.5 times of column volume/h, leave standstill 3h, after using 2 times of column volume deionized waters to carry out wash-out, methyl alcohol-the ethyl acetate (4:1) that re-uses 12 times of column volumes is carried out wash-out, collects methyl alcohol-eluent ethyl acetate liquid;
(7) crystallization and recrystallization: will get dry 595g after step (6) gained elutriant evaporation concentration, the drying, re-use 6kg methyl alcohol-ethyl acetate-acetone (1:1:1) dissolving, and heat to 55 ℃, after keeping this temperature 20min, be cooled to 5 ℃, leave standstill 15h, collect crystal, recrystallization 3 times, drying gets the 505g product.
Detect through liquid phase chromatography, contain linarin 95.40% in the products obtained therefrom.
Embodiment 2
Present embodiment is realized by following steps:
(1) raw materials pretreatment: with 100 kg exsiccant Wild Chrysanthemum removal of impurities, chopping, use 600kg deionized water soak at room temperature 10h, behind the drying water liquid, standby;
(2) potass extraction: use the aqua calcis of 1000kg 2 ‰, under 70 ℃ ~ 80 ℃ condition, soak and extract 3 times, soak 2h at every turn, filter, get extracting solution;
(3) alcohol precipitation: step (2) gained extracting solution evaporation concentration to 149kg, is added 95% ethanol of 400kg then, leave standstill 10h, filter, get pure liquid at 20 ℃;
(4) extraction: to 105kg, the petroleum ether extraction of use 300kg 4 times is collected lower floor's heavy-fluid with step (3) gained alcohol liquid evaporation concentration, and upper strata light liquid petroleum ether layer reclaims;
(5) acid adjustment: step (4) gained heavy-fluid evaporation concentration to 52.5kg, to the hydrochloric acid soln that wherein adds 0.2 mol/L, is regulated pH to 3.5, is cooled to 10 ℃, leave standstill 20h after, the collecting precipitation thing;
(6) absorption with macroporous adsorbent resin separates: step (5) gained throw out is used 70% ethanol (volume) dissolving of 10kg, cross the D101 absorption with macroporous adsorbent resin, the control flow velocity is 1.5 times of column volume/h, leave standstill 3h, use 2 times of column volume deionized waters to carry out wash-out, methyl alcohol-the ethyl acetate (2:1) that re-uses 12 times of column volumes is carried out wash-out, collects methyl alcohol-eluent ethyl acetate liquid;
(7) crystallization and recrystallization: will get dry 564g after step (6) gained elutriant evaporation concentration, the drying, re-use 9kg methyl alcohol-ethyl acetate-acetone (2:2:1) dissolving, and heat to 55 ℃, after keeping this temperature 30min, be cooled to 5 ℃, leave standstill 15h, collect crystal, recrystallization 4 times, drying gets the 475g product.
Detect through liquid phase chromatography, contain linarin 97.67% in the products obtained therefrom.
Embodiment 3
Present embodiment is realized by following steps:
(1) raw materials pretreatment: with 100kg exsiccant Wild Chrysanthemum impurity removing, chopping, use 600kg deionized water soak at room temperature 10h, behind the drying water liquid, standby;
(2) potass extraction: use the sodium carbonate solution of 1000kg 4 ‰, under 70 ℃ ~ 80 ℃ condition, carry soaking and extract 3 times, soak 3h at every turn, filter, get extracting solution;
(3) alcohol precipitation: step (2) gained extracting solution evaporation concentration to 167kg, is added 95% ethanol of 420kg then, leave standstill 10h, filter, get pure liquid at 20 ℃;
(4) extraction: to 107kg, the petroleum ether extraction of use 275kg 3 times is collected lower floor's heavy-fluid with step (3) gained alcohol liquid evaporation concentration, and upper strata light liquid petroleum ether layer reclaims;
(5) acid adjustment: step (4) gained heavy-fluid evaporation concentration to 51.5kg, to the sulphuric acid soln that wherein adds 0.2mol/L, is regulated pH to 4, be cooled to 10 ℃, leave standstill 20h, the collecting precipitation thing;
(6) absorption with macroporous adsorbent resin separates: the dissolve with ethanol 70%(volume that step (5) gained throw out is used 12kg), cross the HPD450 absorption with macroporous adsorbent resin, the control flow velocity is 1.5 times of column volume/h, after leaving standstill 3h, after using 2 times of column volume deionized waters to carry out wash-out, methyl alcohol-the ethyl acetate (2:1) that re-uses 12 times of column volumes is carried out wash-out, collects methyl alcohol-eluent ethyl acetate liquid;
(7) crystallization and recrystallization: will get dry 599g after step (6) elutriant evaporation concentration, the drying, re-use 9kg methyl alcohol-ethyl acetate-acetone (2:2:1) dissolving, and heat to 55 ℃, after keeping this temperature 20min, be cooled to 5 ℃, leave standstill 15h, collect crystal, recrystallization 3 times, drying gets the 487g product.
Detect through liquid phase chromatography, contain linarin 96.18% in the products obtained therefrom.
Embodiment 4
Present embodiment is realized by following steps:
(1) raw materials pretreatment: with the removal of impurities of 100kg exsiccant Wild Chrysanthemum, chopping, use 600kg deionized water soak at room temperature 10h, behind the drying water liquid, standby;
(2) potass extraction: use the sodium hydroxide solution of 1000kg 4 ‰, under 70 ℃ ~ 80 ℃ condition, soak and extract 3 times, soak 3h at every turn, filter, get extracting solution;
(3) alcohol precipitation: step (2) gained extracting solution evaporation concentration to 181kg, is added 95% ethanol of 400kg then, leave standstill 10h, filter, get pure liquid at 20 ℃;
(4) extraction: to 103kg, the petroleum ether extraction of use 300kg 4 times is collected lower floor's heavy-fluid with step (3) gained alcohol liquid evaporation concentration, and upper strata light liquid petroleum ether layer reclaims;
(5) acid adjustment: step (4) gained heavy-fluid evaporation concentration to 43kg, to the sulphuric acid soln that wherein adds 0.2 mol/L, is regulated pH to 3.8, is cooled to 10 ℃, leave standstill 20h after, the collecting precipitation thing;
(6) absorption with macroporous adsorbent resin separates: the dissolve with ethanol 70%(volume that step (5) gained throw out is used 8kg), the control flow velocity is 1.5 times of column volume/h, cross the HPD450 absorption with macroporous adsorbent resin, leave standstill 3h, after using 2 times of column volume deionized waters to carry out wash-out, methyl alcohol-the ethyl acetate (2:1) that re-uses 12 times of column volumes is carried out wash-out, collects methyl alcohol-eluent ethyl acetate liquid;
(7) crystallization and recrystallization: will get dry 613g after step (6) gained elutriant evaporation concentration, the drying, re-use 9.5kg methyl alcohol-ethyl acetate-acetone (1:1:1) dissolving, and heat to 55 ℃, after keeping this temperature 30min, be cooled to 7 ℃, leave standstill 15h, collect crystal, recrystallization 3 times, drying gets the 491g product.
Detect through liquid phase chromatography, contain linarin 96.89% in the products obtained therefrom.
Embodiment 5
Present embodiment is realized by following steps:
(1) raw materials pretreatment: with 100kg exsiccant Wild Chrysanthemum impurity removing, chopping, use 600kg deionized water soak at room temperature 10h, behind the drying water liquid, standby;
(2) potass extraction: the sodium carbonate solution of use 1000kg 3 ‰, under 70 ℃ ~ 80 ℃ conditions, extract to soak and extract 3 times, soak 3h at every turn, filter, get extracting solution;
(3) alcohol precipitation: step (2) gained extracting solution evaporation concentration to 175kg, is added 95% ethanol of 400kg then, leave standstill 10h, filter, get pure liquid at 20 ℃;
(4) extraction: to 110kg, the petroleum ether extraction of use 300kg 3 times is collected lower floor's heavy-fluid with step (3) gained alcohol liquid evaporation concentration, and upper strata light liquid petroleum ether layer reclaims;
(5) acid adjustment: step (4) gained heavy-fluid evaporation concentration to 51.5kg, to the hydrochloric acid soln that wherein adds 0.4 mol/L, is regulated pH to 4.5, is cooled to 10 ℃, leave standstill 20h after, the collecting precipitation thing;
(6) absorption with macroporous adsorbent resin separates: the dissolve with ethanol 70%(volume that step (5) gained throw out is used 7.5kg), cross the D1300 absorption with macroporous adsorbent resin, the control flow velocity is 1.5 times of column volume/h, leave standstill 2h, after using 2 times of column volume deionized waters to carry out wash-out, methyl alcohol-the ethyl acetate (2:1) that re-uses 10 times of column volumes is carried out wash-out, collects methyl alcohol-eluent ethyl acetate liquid;
(7) crystallization and recrystallization: will get dry 644g after step (6) gained elutriant evaporation concentration, the drying, re-use 8.5kg methyl alcohol-ethyl acetate-acetone (1:2:1) dissolving, and heat to 55 ℃, after keeping this temperature 20min, be cooled to 6 ℃, leave standstill 15h, collect crystal, recrystallization 4 times, drying gets the 496g product.
Detect through liquid phase chromatography, contain linarin 96.45% in the products obtained therefrom.
Embodiment 6
Present embodiment is realized by following steps:
(1) raw materials pretreatment: with 100kg exsiccant Wild Chrysanthemum impurity removing, chopping, use 800kg deionized water soak at room temperature 10h, behind the drying water liquid, standby;
(2) potass extraction: use the sodium hydroxide solution of 800,kg5 ‰, under 70 ℃ ~ 80 ℃ condition, carry soaking and extract 3 times, soak 3h at every turn, filter, get extracting solution;
(3) alcohol precipitation: step (2) gained extracting solution evaporation concentration to 157kg, is added 95% ethanol of 350kg then, leave standstill 10h, filter, get pure liquid at 20 ℃;
(4) extraction: to 100.5kg, the petroleum ether extraction of use 300kg 3 times is collected lower floor's heavy-fluid with step (3) gained alcohol liquid evaporation concentration, and upper strata light liquid petroleum ether layer reclaims;
(5) acid adjustment: step (4) gained heavy-fluid evaporation concentration to 48kg, to the phosphoric acid solution that wherein adds 0.4 mol/L, is regulated pH to 3.2, is cooled to 10 ℃, leave standstill 20h after, the collecting precipitation thing;
(6) absorption with macroporous adsorbent resin separates: the dissolve with ethanol 70%(volume that step (5) gained throw out is used 7kg), cross the AB-8 absorption with macroporous adsorbent resin, control flow velocity be 1.5 times of column volumes/hour, leave standstill 2h, after using 2 times of column volume deionized waters to carry out wash-out, methyl alcohol-the ethyl acetate (1:1) that re-uses 12 times of column volumes is carried out wash-out, collects methyl alcohol-eluent ethyl acetate liquid;
(7) crystallization and recrystallization: with after the elutriant evaporation concentration of the above-mentioned gained of step (6), the drying dry 599g, re-use 9kg methyl alcohol-ethyl acetate-acetone (2:1:1) dissolving, and heat to 55 ℃, after keeping this temperature 30min, be cooled to 5 ℃, leave standstill 15h, collect crystal, recrystallization 3 times, drying gets the 483g product.
Detect through liquid phase chromatography, contain linarin 96.37% in the products obtained therefrom.
Claims (8)
1. a method of extracting linarin from Wild Chrysanthemum is characterized in that, comprises the steps:
(1) raw materials pretreatment: with the removal of impurities of exsiccant Wild Chrysanthemum, chopping, use deionized water soak at room temperature 5～10h, behind the drying water liquid, standby;
(2) potass extraction: adding weight is that the mass concentration of 6～10 times of Wild Chrysanthemum raw material dry weights is 2 ‰～8 ‰ alkali aqueous solution, under 70 ℃～80 ℃ condition, soaks and extracts 〉=2 times, soaks 2～3h at every turn, filters, and gets extracting solution;
(3) alcohol precipitation: with step (2) gained extracting solution evaporation concentration to former extracting solution heavy 1/20～1/15, adding weight then is the 95%(volume of 2～3 times of gained concentrated solutions) ethanol, under 20 ℃～30 ℃, leave standstill 6～10h, filter, pure liquid;
(4) extraction: with step (3) gained alcohol liquid evaporation concentration to former gained alcohol liquid measure heavy 1/6～1/5, add weight then and be petroleum ether extraction 〉=2 time of 2～3 times of gained concentrated solutions, collect lower floor's heavy-fluid, upper strata light liquid petroleum ether layer reclaims;
(5) acid adjustment: with step (4) gained heavy-fluid evaporation concentration to its weight 1/3～1/2 after, to the acid solution that wherein adds 0.2～0.4 mol/L, regulate pH to 3～5 after, be cooled to 10 ℃～20 ℃, leave standstill 10～20h, the collecting precipitation thing;
(6) macroporous resin adsorption is separated: is 60%～80% dissolve with ethanol with step (5) gained throw out with being equivalent to 8～12 times of volumetric concentrations of weight of precipitate, last macroporous adsorptive resins, flow velocity is 1.5～2.0 times of column volume/h, leave standstill 2～3h, after using 2～3 times of column volume deionized waters to carry out wash-out, the combination organic solvent that re-uses 8～12 times of column volumes carries out wash-out, collects the organic solvent elutriant;
(7) crystallization and recrystallization: after step (6) gained organic solvent elutriant evaporation concentration, drying, operating weight is the combination organic solvent dissolution of 10～15 times of gained dry-matteies, and heat to 40 ℃～60 ℃, after keeping this temperature 20～30min, be cooled to 5 ℃～10 ℃, leave standstill 10～15h, collect crystal, recrystallization 3～4 times, the dry finished product that gets.
2. the method for extracting linarin from Wild Chrysanthemum according to claim 1, it is characterized in that: described 2 ‰～8 ‰ alkali aqueous solution is sodium hydroxide solution, sodium carbonate solution or aqua calcis.
3. the method for extracting linarin from Wild Chrysanthemum according to claim 1 and 2, it is characterized in that: the acid solution of described 0.2～0.4mol/L is hydrochloric acid, sulfuric acid or phosphoric acid solution.
4. the method for extracting linarin from Wild Chrysanthemum according to claim 1 and 2, it is characterized in that: described macroporous adsorbent resin is D101, D1300, HPD450 or AB-8 macroporous adsorbent resin.
5. the method for extracting linarin from Wild Chrysanthemum according to claim 1 and 2 is characterized in that: described step (6), and used combination organic solvent is methyl alcohol-ethyl acetate mixed solution during wash-out, wherein methyl alcohol and ethyl acetate weight proportion are 2～4:1.
6. the method for extracting linarin from Wild Chrysanthemum according to claim 3 is characterized in that: described step (6), and used combination organic solvent is methyl alcohol-ethyl acetate mixed solution during wash-out, wherein methyl alcohol and ethyl acetate weight proportion are 2～4:1.
7. the method for from Wild Chrysanthemum, extracting linarin according to claim 1 and 2, it is characterized in that: described step (7), used combination organic solvent is methyl alcohol-ethyl acetate-acetone mixed solution during crystallization, and wherein methyl alcohol, ethyl acetate, acetone weight proportion are 1～2:1～2:1.
8. the method for from Wild Chrysanthemum, extracting linarin according to claim 3, it is characterized in that: described step (7), used combination organic solvent is methyl alcohol-ethyl acetate-acetone mixed solution during crystallization, and wherein methyl alcohol, ethyl acetate, acetone weight proportion are 1～2:1～2:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110195580 CN102250172B (en) | 2011-07-13 | 2011-07-13 | Method for extracting Buddleoside from wild chrysanthemum flowers |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110195580 CN102250172B (en) | 2011-07-13 | 2011-07-13 | Method for extracting Buddleoside from wild chrysanthemum flowers |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102250172A true CN102250172A (en) | 2011-11-23 |
| CN102250172B CN102250172B (en) | 2013-08-21 |
Family
ID=44977776
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110195580 Active CN102250172B (en) | 2011-07-13 | 2011-07-13 | Method for extracting Buddleoside from wild chrysanthemum flowers |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102250172B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102706978A (en) * | 2012-06-01 | 2012-10-03 | 北京市药品检验所 | Wild chrysanthemum flower extractive and fingerprint spectrum detection method thereof |
| CN103073605A (en) * | 2012-12-27 | 2013-05-01 | 成都普思生物科技有限公司 | Method for separating and purifying linarin monomers |
| CN103724381A (en) * | 2012-10-15 | 2014-04-16 | 天津药物研究院 | Preparation method of robinin-7-O-rhamnose glucoside and application thereof |
| CN104558071A (en) * | 2013-10-16 | 2015-04-29 | 浙江中医药大学 | Method for extracting and purifying effective part or linarin monomer from chrysantheum indici flos |
| CN104628801A (en) * | 2015-01-21 | 2015-05-20 | 郑州大学 | Process for extracting and separating linarin from wild chrysanthemum |
| CN113354697A (en) * | 2021-07-15 | 2021-09-07 | 广东药科大学 | Method for separating and purifying pectolinarin and linarin |
| CN114014900A (en) * | 2021-11-23 | 2022-02-08 | 湖北工程学院 | Method for extracting and separating linarin from wild chrysanthemum stems |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6442427A (en) * | 1987-08-10 | 1989-02-14 | Tsumura & Co | Sialidase inhibitor |
| CN101857621A (en) * | 2009-04-13 | 2010-10-13 | 上海特善食品科技有限公司 | Preparation method of linarin extracts in wild chrysanthemum flowers |
| CN101955506A (en) * | 2010-05-26 | 2011-01-26 | 南京泽朗医药科技有限公司 | Process for extracting buddleoside |
-
2011
- 2011-07-13 CN CN 201110195580 patent/CN102250172B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6442427A (en) * | 1987-08-10 | 1989-02-14 | Tsumura & Co | Sialidase inhibitor |
| CN101857621A (en) * | 2009-04-13 | 2010-10-13 | 上海特善食品科技有限公司 | Preparation method of linarin extracts in wild chrysanthemum flowers |
| CN101955506A (en) * | 2010-05-26 | 2011-01-26 | 南京泽朗医药科技有限公司 | Process for extracting buddleoside |
Non-Patent Citations (3)
| Title |
|---|
| NIGEL C. VEITCH，等: "Flavonoid glycosides of the black locust tree, Robinia pseudoacacia (Leguminosae)", 《PHYTOCHEMISTRY》 * |
| 冯子明，等: "野菊花的化学成分", 《中国中药杂志》 * |
| 张聪，等: "野菊花的化学成分", 《药学与临床研究》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102706978A (en) * | 2012-06-01 | 2012-10-03 | 北京市药品检验所 | Wild chrysanthemum flower extractive and fingerprint spectrum detection method thereof |
| CN102706978B (en) * | 2012-06-01 | 2013-10-02 | 北京市药品检验所 | Wild chrysanthemum flower extractive and fingerprint spectrum detection method thereof |
| CN103724381A (en) * | 2012-10-15 | 2014-04-16 | 天津药物研究院 | Preparation method of robinin-7-O-rhamnose glucoside and application thereof |
| CN103073605A (en) * | 2012-12-27 | 2013-05-01 | 成都普思生物科技有限公司 | Method for separating and purifying linarin monomers |
| CN103073605B (en) * | 2012-12-27 | 2015-07-08 | 成都普思生物科技有限公司 | Method for separating and purifying linarin monomers |
| CN104558071A (en) * | 2013-10-16 | 2015-04-29 | 浙江中医药大学 | Method for extracting and purifying effective part or linarin monomer from chrysantheum indici flos |
| CN104628801A (en) * | 2015-01-21 | 2015-05-20 | 郑州大学 | Process for extracting and separating linarin from wild chrysanthemum |
| CN113354697A (en) * | 2021-07-15 | 2021-09-07 | 广东药科大学 | Method for separating and purifying pectolinarin and linarin |
| CN113354697B (en) * | 2021-07-15 | 2022-06-28 | 广东药科大学 | Method for separating and purifying pectolinarin and linarin |
| CN114014900A (en) * | 2021-11-23 | 2022-02-08 | 湖北工程学院 | Method for extracting and separating linarin from wild chrysanthemum stems |
| CN114014900B (en) * | 2021-11-23 | 2024-04-16 | 湖北工程学院 | Method for extracting and separating linarin from chrysanthemum indicum stems |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102250172B (en) | 2013-08-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102250172B (en) | Method for extracting Buddleoside from wild chrysanthemum flowers | |
| CN102477056A (en) | Method for purifying neohesperidin | |
| CN109646992B (en) | Method for extracting cannabidiol concentrate from industrial cannabis sativa | |
| CN102190615A (en) | Method for extracting and separating 1-deoxynojirimycin from mulberry leaves | |
| CN101862385B (en) | Sanguisorba saponins and preparation method of sanguisorbin I | |
| CN102701914A (en) | Method for extracting hydroxytyrosol from olive leaves | |
| CN102002083B (en) | Method for extracting high-purity rutin with flash-extraction technology | |
| CN104262251A (en) | Method for extracting huperzine A from serrate clubmoss herb | |
| CN102070684A (en) | Method for extracting syringin | |
| CN101475570B (en) | Method for extracting hypotensor raw material alserin from davilpepper | |
| CN102040637A (en) | Method for extracting sennoside | |
| CN101759731B (en) | Extraction method of linseed gum and secoisolariciresin-ol diglucoside | |
| CN106831930B (en) | A kind of extractant and extracting method for ursolic acid extraction | |
| CN103772457B (en) | Method for preparing geniposidic acid in eucommia leaf | |
| CN102516041A (en) | Method for extracting quebrachitol from natural rubber whey | |
| CN102702287A (en) | Method for extracting purified oleuropein from olive leaves | |
| CN102040611A (en) | Method for extracting mulberry root ketone C | |
| CN102603857A (en) | Method for extracting tea saponin from camellia oleifera cake | |
| CN105111144A (en) | Method of extracting nuciferine from lotus leaves | |
| CN103860626A (en) | Method for preparing total flavonoids in eucommia ulmoides leaves | |
| CN103044410B (en) | A kind of production technique extracting isorientin from bamboo product processing waste material | |
| CN102675106B (en) | Method for preparing high-purity chlorogenic acid by aluminum salt precipitation | |
| CN102002039B (en) | Method for extracting yohimbine from yohimbine bark | |
| CN104478889B (en) | The method of comprehensive utilization of short-tube lycoris resource | |
| CN103467543A (en) | Purification method of moringa oleifera micine |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent of invention or patent application | ||
| CB02 | Change of applicant information |
Address after: 18 floor, Hunan science and technology building, Yuelu Road, Changsha, Hunan, 410000 Applicant after: Hu'nan Huacheng Biological Resources Co., Ltd. Address before: 410000, No. 188 west slope road, Hunan, Changsha, two yards, science and Technology Park, Tongzi Applicant before: Changsha Huacheng Biotech Inc. |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: APPLICANT; FROM: CHANGSHA HUACHENG BIOTECH INC. TO: HU'NAN HUACHENG BIOLOGICAL RESOURCES CO., LTD. |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Method for extracting Buddleoside from wild chrysanthemum flowers Effective date of registration: 20150129 Granted publication date: 20130821 Pledgee: Bank of Beijing Limited by Share Ltd Changsha branch Pledgor: Hu'nan Huacheng Biological Resources Co., Ltd. Registration number: 2015430000002 |
|
| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model | ||
| C56 | Change in the name or address of the patentee | ||
| CP03 | Change of name, title or address |
Address after: Tongzi high tech Zone of Hunan province Changsha Po Road 410205 No. 188 Gold code (Lugu High-tech Park) building two floor West Patentee after: HUNAN HUACHENG BIOTECH, INC. Address before: 18 floor, Hunan science and technology building, Yuelu Road, Changsha, Hunan, 410000 Patentee before: Hu'nan Huacheng Biological Resources Co., Ltd. |
|
| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model | ||
| PM01 | Change of the registration of the contract for pledge of patent right |
Change date: 20160121 Registration number: 2015430000002 Pledgor after: HUNAN HUACHENG BIOTECH, INC. Pledgor before: Hu'nan Huacheng Biological Resources Co., Ltd. |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20160203 Granted publication date: 20130821 Pledgee: Bank of Beijing Limited by Share Ltd Changsha branch Pledgor: HUNAN HUACHENG BIOTECH, INC. Registration number: 2015430000002 |
|
| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Method for extracting Buddleoside from wild chrysanthemum flowers Effective date of registration: 20160222 Granted publication date: 20130821 Pledgee: Bank of Beijing Limited by Share Ltd Changsha branch Pledgor: HUNAN HUACHENG BIOTECH, INC. Registration number: 2016430000003 |
|
| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20170407 Granted publication date: 20130821 Pledgee: Bank of Beijing Limited by Share Ltd Changsha branch Pledgor: HUNAN HUACHENG BIOTECH, INC. Registration number: 2016430000003 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right |