CN102178703A - Method for extracting selaginella biflavone - Google Patents
Method for extracting selaginella biflavone Download PDFInfo
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- CN102178703A CN102178703A CN2011101179975A CN201110117997A CN102178703A CN 102178703 A CN102178703 A CN 102178703A CN 2011101179975 A CN2011101179975 A CN 2011101179975A CN 201110117997 A CN201110117997 A CN 201110117997A CN 102178703 A CN102178703 A CN 102178703A
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- biflavone
- polyethylene glycol
- selaginella
- selaginella tamariscina
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Abstract
The invention relates to a method for extracting selaginella biflavone, and belongs to the technical field of chemical extraction process of medicinal plants. The method comprises the following steps of: extracting selaginella serving as a raw material by using petroleum ether and acetone sequentially, adding acetone extracting solution into inorganic salt solution and polyethylene glycol, stirring, mixing fully for extracting, and standing to form two phases; and allowing selaginella biflavone to enter a polyethylene glycol top phase, separating the selaginella biflavone from polyethylene glycol by top phase liquid through an ultrafiltration membrane method, concentrating the selaginella biflavone by using a nanofiltration membrane, reconcentrating and drying to obtain a selaginella biflavone product. In the method, the technology of two aqueous phase extraction and membrane concentration is adopted, so the method adopts a simple extraction process and has low requirement on equipment, and is suitable for industrial production.
Description
Technical field:
The present invention relates to a kind of method of extracting selaginella tamariscina biflavone.
Background technology:
Rock lily plant is widely distributed, kind surplus the whole world has 700, kind surplus China has 70.Modern pharmacological research shows that Rock lily plant not only has traditional eliminating inflammation and expelling toxin effect, and has blood pressure lowering, blood sugar lowering, antibiotic, antiviral, raise immunity and inhibited oxidation and stress wait effect.The chemical constituent of Selaginella is flavonoid, alkaloid, phenols, organic acid, aminoacid and polysaccharide etc., and is the highest based on the bis-flavonoid content of amentoflavone.Chinese patent application number 200810197033.4 disclosed methods are for to dry the Herba Selaginellae Involventis vegetable material, roguing, pulverize, with the petroleum ether defat that refluxes, reuse 40%-95% alcoholic solution reflux, extract,, filter, solvent is reclaimed in the filtrate evaporation, and residue is with ethyl acetate extraction, and extract reclaims the solvent after drying, get ethyl acetate extract, this extract is dissolved in the 5%-45% alcoholic solution, uses purification by macroporous resin, collect suitable flow point, reclaim the ethanol after drying, obtain the total bisflavone extract of Herba Selaginellae Involventis.This method is used a large amount of organic solvents, and dissolvent residual is many, and the macroporous resin adsorption adsorption effect is undesirable, and sample loss is bigger.Chinese patent application numbers 200910066695.2 provides a kind of preparation method of selaginella tamariscina biflavone ingredient, utilize ethanol extraction and polyamide column chromatography method from the cushion volume plant, a large amount of preparation high-load Herba Selaginellae total flavones and high-purity amentoflavone monomer components Herba Selaginellae and the Herba Selaginellae Involventis.This method directly goes up the polyamide column adsorption and purification without concentrating, and greatly reduces the adsorption effect of resin column.
Summary of the invention:
The industrialization of selaginella tamariscina biflavone is extracted most important, for filling up the deficiency of existing extraction process, the invention provides a kind of method of extracting selaginella tamariscina biflavone.
The objective of the invention is to realize by following concrete technical scheme:
A kind of method of extracting selaginella tamariscina biflavone, it is characterized in that: be raw material with the Herba Selaginellae, use petroleum ether, acetone extraction successively, acetone extract adds inorganic salt solution and Polyethylene Glycol, stirs, make abundant hybrid extraction, it is biphase to leave standstill back formation, and selaginella tamariscina biflavone enters phase on the Polyethylene Glycol, and last phase liquid adopts ultrafiltrationmembrane process that selaginella tamariscina biflavone is separated with Polyethylene Glycol, selaginella tamariscina biflavone adopts NF membrane to concentrate, and reconcentration, drying obtain the selaginella tamariscina biflavone product.
Described inorganic salt is the one or more combination in ammonium sulfate, sodium sulfate, potassium carbonate, potassium dihydrogen phosphate, the dipotassium hydrogen phosphate.
The relative molecular weight of described Polyethylene Glycol is 4000 or 6000, and the mass concentration of Polyethylene Glycol is 15-30% in the double-aqueous phase system, and the mass concentration of inorganic salt is 10-15%, and extraction temperature is 20-35 ℃, and described time of repose is 10-15 hour.
The molecular cut off of described ultrafilter membrane is 2000-4000, and the molecular cut off of described NF membrane is below 300.
Compared with prior art, (1) the present invention adopts aqueous two-phase extraction that bisflavone is separated with alkaloid, polysaccharide impurity; (2) adopt embrane method to concentrate, can significantly cut down the consumption of energy; (3) extraction process of the present invention is simple, equipment requirements is low, cost is low, pollution-free, be fit to industrialization production.
The specific embodiment:
Embodiment 1:
Take by weighing 80 order Spikemoss 200g, add the 1600ml petroleum ether and carry out the Soxhlet extraction, extracting temperature is 60-90 ℃, extraction time is 1h, and raffinate vapors away residual petroleum ether, gets the petroleum ether raffinate, raffinate is measured the acetone heating and refluxing extraction with 10 times, repeat 2 times, merge extractive liquid,, rotary evaporation concentrate and obtain the acetone concentrated solution; The pH that adjusts the acetone concentrated solution is 3.5, add polyethylene glycol 6000 and ammonium sulfate successively, the mass concentration that makes Polyethylene Glycol in the formed two phase aqueous extraction system is 15%, the mass concentration of ammonium sulfate is 12%, stir under 25 ℃ of temperature and extract half an hour, leave standstill then and formed biphase in 10 hours, selaginella tamariscina biflavone enters phase on the Polyethylene Glycol, adopting molecular cut off is that 4000 ultrafilter membrane will contain selaginella tamariscina biflavone and obtain separating mutually on the Polyethylene Glycol, collect the permeate selaginella tamariscina biflavone, adopt NF membrane that the selaginella tamariscina biflavone permeate is concentrated, concentrated solution is further concentrated under vacuum, drying obtains the selaginella tamariscina biflavone powder, and general flavone content reaches more than 65% in amentoflavone.
Embodiment 2:
Take by weighing 40 order Spikemoss 200g, add the 1400ml petroleum ether and carry out the Soxhlet extraction, extracting temperature is 60-90 ℃, extraction time is 2h, and raffinate vapors away residual petroleum ether, gets the petroleum ether raffinate, raffinate is measured the acetone heating and refluxing extraction with 8 times, repeat 3 times, merge extractive liquid,, rotary evaporation concentrate and obtain the acetone concentrated solution; The pH that adjusts the acetone concentrated solution is 4.0, add Macrogol 4000 and sodium sulfate successively, the mass concentration that makes Polyethylene Glycol in the formed two phase aqueous extraction system is 30%, the mass concentration of sodium sulfate is 13%, stir under 30 ℃ of temperature and extract half an hour, leave standstill then and formed biphase in 13 hours, selaginella tamariscina biflavone enters phase on the Polyethylene Glycol, adopting molecular cut off is that 2000 ultrafilter membrane will contain selaginella tamariscina biflavone and obtain separating mutually on the Polyethylene Glycol, collect the permeate selaginella tamariscina biflavone, adopt NF membrane that the selaginella tamariscina biflavone permeate is concentrated, concentrated solution is further concentrated under vacuum, drying obtains the selaginella tamariscina biflavone powder, and general flavone content reaches more than 65% in amentoflavone.
Embodiment 3:
Take by weighing 40 order Spikemoss 200g, add the 2000ml petroleum ether and carry out the Soxhlet extraction, extracting temperature is 60-90 ℃, extraction time is 2h, and raffinate vapors away residual petroleum ether, gets the petroleum ether raffinate, raffinate is measured the acetone heating and refluxing extraction with 12 times, repeat 2 times, merge extractive liquid,, rotary evaporation concentrate and obtain the acetone concentrated solution; The pH that adjusts the acetone concentrated solution is 3.0, add polyethylene glycol 6000 and potassium carbonate successively, the mass concentration that makes Polyethylene Glycol in the formed two phase aqueous extraction system is 25%, the mass concentration of potassium carbonate is 15%, stir under 28 ℃ of temperature and extract half an hour, leave standstill then and formed biphase in 12 hours, selaginella tamariscina biflavone enters phase on the Polyethylene Glycol, adopting molecular cut off is that 3000 ultrafilter membrane will contain selaginella tamariscina biflavone and obtain separating mutually on the Polyethylene Glycol, collect the permeate selaginella tamariscina biflavone, adopt NF membrane that the selaginella tamariscina biflavone permeate is concentrated, concentrated solution is further concentrated under vacuum, drying obtains the selaginella tamariscina biflavone powder, and general flavone content reaches more than 65% in amentoflavone.
Embodiment 4:
Take by weighing 60 order Spikemoss 200g, add the 1800ml petroleum ether and carry out the Soxhlet extraction, extracting temperature is 60-90 ℃, extraction time is 1.5h, and raffinate vapors away residual petroleum ether, gets the petroleum ether raffinate, raffinate is measured the acetone heating and refluxing extraction with 6 times, repeat 2 times, merge extractive liquid,, rotary evaporation concentrate and obtain the acetone concentrated solution; The pH that adjusts the acetone concentrated solution is 3.0, add polyethylene glycol 6000 and potassium dihydrogen phosphate successively, the mass concentration that makes Polyethylene Glycol in the formed two phase aqueous extraction system is 15%, the mass concentration of potassium dihydrogen phosphate is 10%, stir under 20 ℃ of temperature and extract half an hour, leave standstill then and formed biphase in 15 hours, selaginella tamariscina biflavone enters phase on the Polyethylene Glycol, adopting molecular cut off is that 2000 ultrafilter membrane will contain selaginella tamariscina biflavone and obtain separating mutually on the Polyethylene Glycol, collect the permeate selaginella tamariscina biflavone, adopt NF membrane that the selaginella tamariscina biflavone permeate is concentrated, concentrated solution is further concentrated under vacuum, drying obtains the selaginella tamariscina biflavone powder, and general flavone content reaches more than 65% in amentoflavone.
Embodiment 5:
Take by weighing 20 order Spikemoss 200g, add the 1500ml petroleum ether and carry out the Soxhlet extraction, extracting temperature is 60-90 ℃, extraction time is 3h, and raffinate vapors away residual petroleum ether, gets the petroleum ether raffinate, raffinate is measured the acetone heating and refluxing extraction with 12 times, repeat 3 times, merge extractive liquid,, rotary evaporation concentrate and obtain the acetone concentrated solution; The pH that adjusts the acetone concentrated solution is 4, add Macrogol 4000 and dipotassium hydrogen phosphate successively, the mass concentration that makes Polyethylene Glycol in the formed two phase aqueous extraction system is 20%, the mass concentration of dipotassium hydrogen phosphate is 11%, stir under 35 ℃ of temperature and extract half an hour, leave standstill then and formed biphase in 14 hours, selaginella tamariscina biflavone enters phase on the Polyethylene Glycol, adopting molecular cut off is that 3000 ultrafilter membrane will contain selaginella tamariscina biflavone and obtain separating mutually on the Polyethylene Glycol, collect the permeate selaginella tamariscina biflavone, adopt NF membrane that the selaginella tamariscina biflavone permeate is concentrated, concentrated solution is further concentrated under vacuum, drying obtains the selaginella tamariscina biflavone powder, and general flavone content reaches more than 65% in amentoflavone.
Claims (4)
1. method of extracting selaginella tamariscina biflavone, it is characterized in that: be raw material with the Herba Selaginellae, use petroleum ether, acetone extraction successively, acetone extract adds inorganic salt solution and Polyethylene Glycol, stirs, make abundant hybrid extraction, it is biphase to leave standstill back formation, and selaginella tamariscina biflavone enters phase on the Polyethylene Glycol, and last phase liquid adopts ultrafiltrationmembrane process that selaginella tamariscina biflavone is separated with Polyethylene Glycol, selaginella tamariscina biflavone adopts NF membrane to concentrate, and reconcentration, drying obtain the selaginella tamariscina biflavone product.
2. method according to claim 1 is characterized in that: described inorganic salt is the one or more combination in ammonium sulfate, sodium sulfate, potassium carbonate, potassium dihydrogen phosphate, the dipotassium hydrogen phosphate.
3. method according to claim 1, it is characterized in that: the relative molecular weight of described Polyethylene Glycol is 4000 or 6000, the mass concentration of Polyethylene Glycol is 15-30% in the double-aqueous phase system, the mass concentration of inorganic salt is 10-15%, extraction temperature is 20-35 ℃, and described time of repose is 10-15 hour.
4. method according to claim 1 is characterized in that: the molecular cut off of described ultrafilter membrane is 2000-4000, and the molecular cut off of described NF membrane is below 300.
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| CN2011101179975A CN102178703A (en) | 2011-05-06 | 2011-05-06 | Method for extracting selaginella biflavone |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102319282A (en) * | 2011-09-21 | 2012-01-18 | 武汉工程大学 | Aqueous two-phase extraction method for total flavones in kudzu root |
| CN102697839A (en) * | 2012-06-01 | 2012-10-03 | 武汉工程大学 | Aqueous two-phase extraction and separation method for flavonoids, saponins and polysaccharides of astragalus |
| CN102911030A (en) * | 2011-08-02 | 2013-02-06 | 苏州宝泽堂医药科技有限公司 | Aqueous two-phase extraction method of angelica keiskei chalcone |
| CN103083379A (en) * | 2013-02-28 | 2013-05-08 | 中国人民解放军兰州军区乌鲁木齐总医院 | Preparation method and application of snow chrysanthemum flavonoids |
| CN111217864A (en) * | 2020-02-28 | 2020-06-02 | 营山椒宝宝花椒有限责任公司 | Extraction method of green pepper alkaloid |
| CN112194721A (en) * | 2019-10-29 | 2021-01-08 | 西北农林科技大学 | Double-solution mixed extraction system and application thereof in ostrich liver |
| CN114814057A (en) * | 2022-04-28 | 2022-07-29 | 湖南省药品检验检测研究院 | Method for distinguishing true and false of selaginella tamariscina varieties through non-targeted metabonomics and application |
-
2011
- 2011-05-06 CN CN2011101179975A patent/CN102178703A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102911030A (en) * | 2011-08-02 | 2013-02-06 | 苏州宝泽堂医药科技有限公司 | Aqueous two-phase extraction method of angelica keiskei chalcone |
| CN102319282A (en) * | 2011-09-21 | 2012-01-18 | 武汉工程大学 | Aqueous two-phase extraction method for total flavones in kudzu root |
| CN102319282B (en) * | 2011-09-21 | 2013-07-10 | 武汉工程大学 | Aqueous two-phase extraction method for total flavones in kudzu root |
| CN102697839A (en) * | 2012-06-01 | 2012-10-03 | 武汉工程大学 | Aqueous two-phase extraction and separation method for flavonoids, saponins and polysaccharides of astragalus |
| CN102697839B (en) * | 2012-06-01 | 2014-04-09 | 武汉工程大学 | Aqueous two-phase extraction and separation method for flavonoids, saponins and polysaccharides of astragalus |
| CN103083379A (en) * | 2013-02-28 | 2013-05-08 | 中国人民解放军兰州军区乌鲁木齐总医院 | Preparation method and application of snow chrysanthemum flavonoids |
| CN112194721A (en) * | 2019-10-29 | 2021-01-08 | 西北农林科技大学 | Double-solution mixed extraction system and application thereof in ostrich liver |
| CN112194721B (en) * | 2019-10-29 | 2022-12-23 | 西北农林科技大学 | Double-solution mixed extraction system and application thereof in ostrich liver |
| CN111217864A (en) * | 2020-02-28 | 2020-06-02 | 营山椒宝宝花椒有限责任公司 | Extraction method of green pepper alkaloid |
| CN111217864B (en) * | 2020-02-28 | 2020-10-27 | 营山椒宝宝花椒有限责任公司 | Extraction method of green pepper alkaloid |
| CN114814057A (en) * | 2022-04-28 | 2022-07-29 | 湖南省药品检验检测研究院 | Method for distinguishing true and false of selaginella tamariscina varieties through non-targeted metabonomics and application |
| CN114814057B (en) * | 2022-04-28 | 2024-01-16 | 湖南省药品检验检测研究院 | Method for distinguishing true and false of selaginella tamariscina varieties by non-targeted metabonomics and application |
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Application publication date: 20110914 |