CN102250172B - Method for extracting Buddleoside from wild chrysanthemum flowers - Google Patents
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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 that the Wild Chrysanthemum with drying is raw material, 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 Wild Chrysanthemum removal of impurities, the chopping of drying, 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, get 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: be 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
Be described in further detail below in conjunction with the present invention of embodiment.
Embodiment 1
Present embodiment is realized by following steps:
(1) raw materials pretreatment: with Wild Chrysanthemum removal of impurities, the chopping of 100 kg dryings, 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 Wild Chrysanthemum removal of impurities, the chopping of 100 kg dryings, 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 at 20 ℃, filter, get pure liquid;
(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 Wild Chrysanthemum impurity removing, the chopping of 100kg drying, 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 at 20 ℃, filter, get pure liquid;
(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 Wild Chrysanthemum removal of impurities, the chopping of 100kg drying, 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 at 20 ℃, filter, get pure liquid;
(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 Wild Chrysanthemum impurity removing, the chopping of 100kg drying, 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 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 at 20 ℃, filter, get pure liquid;
(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 Wild Chrysanthemum impurity removing, the chopping of 100kg drying, 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 at 20 ℃, filter, get pure liquid;
(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 (4)
1. a method of extracting linarin from Wild Chrysanthemum is characterized in that, comprises the steps:
(1) raw materials pretreatment: with Wild Chrysanthemum removal of impurities, the chopping of drying, 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, get 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: be 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;
Described combination organic solvent is methyl alcohol-ethyl acetate mixed solution, and wherein methyl alcohol and ethyl acetate weight proportion are 2 ~ 4:1;
(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;
Described combination organic solvent is methyl alcohol-ethyl acetate-acetone mixed solution, and wherein methyl alcohol, ethyl acetate, acetone weight proportion are 1 ~ 2:1 ~ 2:1.
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.
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Families Citing this family (8)
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| 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 |
| 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 |
| CN104628801B (en) * | 2015-01-21 | 2017-06-16 | 郑州大学 | One kind is extracted from chrysanthemum indicum and separates linarin technique |
| CN113354697B (en) * | 2021-07-15 | 2022-06-28 | 广东药科大学 | Method for separating and purifying pectolinarin and linarin |
| CN114014900B (en) * | 2021-11-23 | 2024-04-16 | 湖北工程学院 | Method for extracting and separating linarin from chrysanthemum indicum stems |
| CN115594726A (en) * | 2022-10-24 | 2023-01-13 | 湖北华龙生物制药有限公司（Cn） | Optimized process for extracting linarin from wild chrysanthemum flowers |
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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 |
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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. |
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Change date: 20160121 Registration number: 2015430000002 Pledgor after: HUNAN HUACHENG BIOTECH, INC. Pledgor before: Hu'nan Huacheng Biological Resources Co., Ltd. |
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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 |
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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 |
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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 |
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