CN103450136A - Method for extracting hinokiflavone from Cacumen Biotae - Google Patents
Method for extracting hinokiflavone from Cacumen Biotae Download PDFInfo
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- CN103450136A CN103450136A CN 201310360308 CN201310360308A CN103450136A CN 103450136 A CN103450136 A CN 103450136A CN 201310360308 CN201310360308 CN 201310360308 CN 201310360308 A CN201310360308 A CN 201310360308A CN 103450136 A CN103450136 A CN 103450136A
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Abstract
The invention discloses a method for extracting hinokiflavone from Cacumen Biotae. The method comprises the following steps: 1) pulverizing Cacumen Biotae, adding 5-10 times of saturated lime water for immersion and extraction for 2-3 times, ultrafiltering the extracting solution through an ultrafiltration membrane, and concentrating the filtrate with a nanofiltration membrane to obtain a concentrated solution; 2) regulating the pH value of the concentrated solution to 3-5, adding into a macroporous resin column for adsorption, carrying out gradient elution with an ethanol solution, concentrating the eluate, regulating the pH value to 3-5, and crystallizing; and 3) dissolving the filtered crystal in a 50-80% methanol solution, concentrating until the methanol concentration is 10-30%, adding into a macroporous resin for adsorption, carrying out gradient elution with an ethanol solution, concentrating the eluate for crystallization, recrystallizing the crystal with a 70% ethanol solution, and drying. The method for producing hinokiflavone has the advantages of simple technological operation, low energy consumption and small pollution, and can easily implement industrial production.
Description
Technical field
The invention belongs to biological technical field, be specifically related to a kind of method of extracting hinokiflavone from Leafy twigs of Oriental Arborvitae.
Background technology
Hinokiflavone is Flavonoid substances, and CAS numbers 19202-36-9, fusing point 353-355 °, and molecular weight is C30H18O10, molecular weight is 538.47.Molecular structural formula:
Modern study finds that hinokiflavone has anti-inflammatory, the effect such as antibiotic and antitumor.
By literature search, the hinokiflavone preparation method adopts chromatography more, and as patent " a kind of preparation method of hinokiflavone ", the disclosed method of this patent is to adopt the polymeric amide chromatographic column to separate.This class methods reagent dosage is large, and the purge process complexity is difficult to realize suitability for industrialized production.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of easy and simple to handle method of hinokiflavone of extracting from Selaginella tamariscina.
The present invention is achieved by the following technical solutions:
A kind of method of extracting hinokiflavone from Leafy twigs of Oriental Arborvitae is characterized in that comprising the following steps:
1) get the Leafy twigs of Oriental Arborvitae pulverizing and add 5-10 doubly to measure saturated limewater immersion extraction 2-3 time, extracting solution adds the ultra-filtration membrane ultrafiltration, sees through liquid concentrated by nanofiltration membrane again, obtains concentrated solution;
2) add in macroporous resin column after concentrated solution adjusting ph to 3-5 and adsorb, the ethanolic soln gradient elution, the concentrated adjusting of elutriant ph3-5 crystallization,
3) leach crystallization 50%-80% dissolve with methanol solution, be concentrated into determining alcohol to 10%-30%, add macroporous resin adsorption, the ethanolic soln gradient elution, the elutriant condensing crystal, crystallisate is used 70% ethanolic soln recrystallization again, is drying to obtain.
The hollow cellulose film that ultra-filtration membrane in described step 1) is molecular weight cut-off 3000-10000, the hollow cellulose film that nanofiltration membrane is molecular weight cut-off 100-500.
Described step 2) and 3) macroporous resin in be a kind of in D101, AB-8, HPD100 and HZ816.
Described step 2) and 3) ethanol gradient elution be: first get 5-10 times of column volume 20%-40% ethanolic soln wash-out impurity, then by 5-10 times of column volume 50%-80% ethanol elution effective constituent.
Adopt technique scheme to produce hinokiflavone, technique is simple to operation, and energy consumption is low, is easy to realize suitability for industrialized production.
Embodiment
below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1:
Getting the pulverizing of 20kg Leafy twigs of Oriental Arborvitae adds 10 times of amount saturated limewaters to soak extraction 2 times, extracting solution filters the hollow cellulose membrane ultrafiltration that adds molecular weight cut-off 3000, see through liquid and use again the hollow cellulose membrane concentration of molecular weight cut-off 500, add in the D101 macroporous resin column and adsorb after concentrated solution adjusting ph to 5, first get 5 times of column volumes, 20% ethanolic soln wash-out impurity, use again 10 times of column volumes, 50% ethanol elution effective constituent, the concentrated adjusting of elutriant ph3 crystallization.Leaching crystallization dissolves with 80% methanol eddy, be concentrated into determining alcohol to 10%, add in the D101 macroporous resin column and adsorb, first get 5 times of column volumes, 30% ethanolic soln wash-out impurity, then use 7 times of column volumes, 60% ethanol elution effective constituent, the elutriant condensing crystal, crystallisate is used 70% ethanolic soln recrystallization again, and drying obtains hinokiflavone 28g, detect content 98.5% through HPLC.
Embodiment 2:
Getting the pulverizing of 20kg Leafy twigs of Oriental Arborvitae adds 5 times of amount saturated limewaters to soak extraction 3 times, extracting solution filters the hollow cellulose membrane ultrafiltration that adds molecular weight cut-off 6000, see through liquid and use again the hollow cellulose membrane concentration of molecular weight cut-off 400, add in the AB-8 macroporous resin column and adsorb after concentrated solution adjusting ph to 5, first get 6 times of column volumes, 30% ethanolic soln wash-out impurity, use again 7 times of column volumes, 60% ethanol elution effective constituent, the concentrated adjusting of elutriant ph4 crystallization.Leaching crystallization dissolves with 50% methanol eddy, be concentrated into determining alcohol to 20%, add in the AB-8 macroporous resin column and adsorb, first get 10 times of column volumes, 20% ethanolic soln wash-out impurity, then use 7 times of column volumes, 65% ethanol elution effective constituent, the elutriant condensing crystal, crystallisate is used 70% ethanolic soln recrystallization again, and drying obtains hinokiflavone 32g, detect content 98.8% through HPLC.
Embodiment 3:
Getting the pulverizing of 20kg Leafy twigs of Oriental Arborvitae adds 5 times of amount saturated limewaters to soak extraction 3 times, extracting solution filters the hollow cellulose membrane ultrafiltration that adds molecular weight cut-off 6000, see through liquid and use again the hollow cellulose membrane concentration of molecular weight cut-off 400, add in the HZ816 macroporous resin column and adsorb after concentrated solution adjusting ph to 5, first get 6 times of column volumes, 30% ethanolic soln wash-out impurity, use again 7 times of column volumes, 60% ethanol elution effective constituent, the concentrated adjusting of elutriant ph4 crystallization.Leaching crystallization dissolves with 50% methanol eddy, be concentrated into determining alcohol to 10%, add in the HZ816 macroporous resin column and adsorb, first get 6 times of column volumes, 20% ethanolic soln wash-out impurity, then use 7 times of column volumes, 60% ethanol elution effective constituent, the elutriant condensing crystal, crystallisate is used 70% ethanolic soln recrystallization again, and drying obtains hinokiflavone 29g, detect content 98.1% through HPLC.
Embodiment 4:
Getting the pulverizing of 20kg Leafy twigs of Oriental Arborvitae adds 5 times of amount saturated limewaters to soak extraction 3 times, extracting solution filters the hollow cellulose membrane ultrafiltration that adds molecular weight cut-off 3000, see through liquid and use again the hollow cellulose membrane concentration of molecular weight cut-off 300, add in the HPD100 macroporous resin column and adsorb after concentrated solution adjusting ph to 5, first get 6 times of column volumes, 30% ethanolic soln wash-out impurity, use again 7 times of column volumes, 60% ethanol elution effective constituent, the concentrated adjusting of elutriant ph4 crystallization.Leaching crystallization dissolves with 50% methanol eddy, be concentrated into determining alcohol to 20%, add in the HPD100 macroporous resin column and adsorb, first get 5 times of column volumes, 20% ethanolic soln wash-out impurity, then use 7 times of column volumes, 60% ethanol elution effective constituent, the elutriant condensing crystal, crystallisate is used 70% ethanolic soln recrystallization again, and drying obtains hinokiflavone 28g, detect content 98.5% through HPLC.
Claims (4)
1. a method of extracting hinokiflavone from Leafy twigs of Oriental Arborvitae is characterized in that comprising the following steps:
1) get the Leafy twigs of Oriental Arborvitae pulverizing and add 5-10 doubly to measure saturated limewater immersion extraction 2-3 time, extracting solution adds the ultra-filtration membrane ultrafiltration, sees through liquid concentrated by nanofiltration membrane again, obtains concentrated solution;
2) add in macroporous resin column after concentrated solution adjusting ph to 3-5 and adsorb, the ethanolic soln gradient elution, the concentrated adjusting of elutriant ph3-5 crystallization,
3) leach crystallization 50%-80% dissolve with methanol solution, be concentrated into determining alcohol to 10%-30%, add macroporous resin adsorption, the ethanolic soln gradient elution, the elutriant condensing crystal, crystallisate is used 70% ethanolic soln recrystallization again, is drying to obtain.
2. the method for extracting hinokiflavone from Leafy twigs of Oriental Arborvitae according to claim 1, it is characterized in that the hollow cellulose film that the ultra-filtration membrane in described step 1) is molecular weight cut-off 3000-10000, the hollow cellulose film that nanofiltration membrane is molecular weight cut-off 100-500.
3. the method for extracting hinokiflavone from Leafy twigs of Oriental Arborvitae according to claim 1, is characterized in that described step 2) and 3) macroporous resin in be a kind of in D101, AB-8, HPD100 and HZ816.
4. the method for extracting hinokiflavone from Leafy twigs of Oriental Arborvitae according to claim 1, it is characterized in that described step 2) and 3) ethanol gradient elution be: first get 5-10 times of column volume 20%-40% ethanolic soln wash-out impurity, then by 5-10 times of column volume 50%-80% ethanol elution effective constituent.
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| CN 201310360308 CN103450136A (en) | 2013-08-19 | 2013-08-19 | Method for extracting hinokiflavone from Cacumen Biotae |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104546952A (en) * | 2014-12-10 | 2015-04-29 | 福建医科大学 | Active component of selaginella doederleinii hieron as well as preparation method and use thereof |
| CN105486647A (en) * | 2015-09-29 | 2016-04-13 | 吉林农业大学 | Extraction and performance determination for hair-blackening active composition in cacumen platycladi |
| CN105566271A (en) * | 2015-12-03 | 2016-05-11 | 福建医科大学 | Biflavone compound and application thereof to preparation of medicine for treating cancer |
| CN105622561A (en) * | 2015-12-24 | 2016-06-01 | 杭州研谱科技有限公司 | Method for extracting podocar-pusflavone from juniper berry meal |
| CN107216301A (en) * | 2017-05-23 | 2017-09-29 | 芜湖欧标农业发展有限公司 | A kind of preparation method of efficient hinokiflavone |
| CN109824638A (en) * | 2019-04-01 | 2019-05-31 | 山东笑康生物科技有限公司 | A method of the Ti Qu Ash skin ketone from cortex dictamni |
-
2013
- 2013-08-19 CN CN 201310360308 patent/CN103450136A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104546952A (en) * | 2014-12-10 | 2015-04-29 | 福建医科大学 | Active component of selaginella doederleinii hieron as well as preparation method and use thereof |
| CN104546952B (en) * | 2014-12-10 | 2018-02-06 | 福建医科大学 | A kind of selaginella doederlleini active component and its production and use |
| CN105486647A (en) * | 2015-09-29 | 2016-04-13 | 吉林农业大学 | Extraction and performance determination for hair-blackening active composition in cacumen platycladi |
| CN105486647B (en) * | 2015-09-29 | 2019-07-19 | 吉林农业大学 | The extraction and performance measurement of black hair active constituent in cacumen biotae |
| CN105566271A (en) * | 2015-12-03 | 2016-05-11 | 福建医科大学 | Biflavone compound and application thereof to preparation of medicine for treating cancer |
| CN105566271B (en) * | 2015-12-03 | 2019-09-13 | 福建医科大学 | The purposes of biflavone compound and its drug of preparation treating cancer |
| CN105622561A (en) * | 2015-12-24 | 2016-06-01 | 杭州研谱科技有限公司 | Method for extracting podocar-pusflavone from juniper berry meal |
| CN105622561B (en) * | 2015-12-24 | 2018-02-16 | 杭州研谱科技有限公司 | A kind of method that podocarpusflavone is extracted in the fruit dregs of rice from needle juniper |
| CN107216301A (en) * | 2017-05-23 | 2017-09-29 | 芜湖欧标农业发展有限公司 | A kind of preparation method of efficient hinokiflavone |
| CN109824638A (en) * | 2019-04-01 | 2019-05-31 | 山东笑康生物科技有限公司 | A method of the Ti Qu Ash skin ketone from cortex dictamni |
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