CN102232993A - Method for extracting general flavone from herba desmodii styracifolii - Google Patents
Method for extracting general flavone from herba desmodii styracifolii Download PDFInfo
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- CN102232993A CN102232993A CN2011101178686A CN201110117868A CN102232993A CN 102232993 A CN102232993 A CN 102232993A CN 2011101178686 A CN2011101178686 A CN 2011101178686A CN 201110117868 A CN201110117868 A CN 201110117868A CN 102232993 A CN102232993 A CN 102232993A
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- herba desmodii
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Abstract
The invention relates to a method for extracting general flavone from herba desmodii styracifolii, in particular to a preparation process for extracting the purified general flavone from the herba desmodii styracifolii. The method comprises the following process steps of: taking herba desmodii styracifolii medicinal materials, adding low-carbon alcohols into the herba desmodii styracifolii medicinal materials for reflowing and extracting; condensing an extraction solution to be small volume; standing and removing precipitation; removing water-soluble macromolecules by using an ultrafiltration membrane; feeding macroporous resin and adsorbing; and eluting with an alcohol solution and collecting the general flavone of the herba desmodii styracifoli. The method has the advantages of simpleness in operation, low requirement for equipment, higher purity of the obtained product, and the like.
Description
Technical field:
The invention belongs to the Separation of Natural Products field, specifically relate to a kind of method of from Herba Desmodii Styracifolii, extracting total flavones, particularly adopt the method for membrance separation in conjunction with purification by macroporous resin Herba Desmodii Styracifolii total flavones.
Background technology:
Herba Desmodii Styracifolii (Desmodium styracifolium (Osbeck) Merr.) is a pulse family beggar-ticks plant, abound with in Guangxi, ground such as Guangdong, Fujian, its nature and flavor are sweet, light, cool, be China's Chinese medicine commonly used, have heat clearing away, diuresis, urinary calculus removing function, be used for urinary system infection, urinary system calculus, cholelithiasis, acute icterohepatitis etc., contain flavonoid, alkaloids, saponins, compositions such as phenols.Pharmacological research proves: the effect that the rat calcium oxalate lithangiuria that the flavonoid glycoside compound in the Herba Desmodii Styracifolii has prevention ethylene glycol and vitamin D to cause forms, the Herba Desmodii Styracifolii total flavones has good improvement effect to cardiovascular and cerebrovascular vessel pathology model.
At present, the extraction of Herba Desmodii Styracifolii total flavones is limited to the extraction research to its crude extract more, is further purified work.Wang Xiaolin etc. disclosed " technical study of ultrasound wave assisted extraction Herba Desmodii Styracifolii total flavones ", the method that the document adopts is: adopt 20 times of amount 70% ethanol ultrasonic extraction 3 times, each 30min obtain extracting total flavones completely, but the document is not further purified processing to it.Document " in the Herba Desmodii Styracifolii total flavone extracting process research ", the optimised process that the document is determined is: 15 times of water gaging reflux, extract, 3 times, each 1.5h, this method is not further purified total flavones equally.
Summary of the invention:
The purpose of this invention is to provide a kind of method of extracting total flavones from Herba Desmodii Styracifolii, this method is easy and simple to handle, environmentally safe, and energy consumption is relatively little, and the purity of the total flavones that makes is higher.
A kind of method of extracting total flavones from Herba Desmodii Styracifolii is characterized in that the method includes the steps of:
1) with the Herba Lysimachiae pulverizing medicinal materials, be added to and extract in the still, adopt 50～70% low-carbon alcohols reflux, extract,, extracting solution places the vacuum concentration still, is concentrated into 1/2～2/3 of former extracting liquid volume, leaves standstill, and isolates supernatant;
2) with above-mentioned supernatant thin up, cross ultrafilter membrane and carry out ultrafiltration, remove water-soluble macromolecule and get hyperfiltration treatment liquid.
3) get macroporous resin wet method dress post, above-mentioned hyperfiltration treatment liquid slowly fed resin column, first water eluting impurity, reuse ethanol liquid eluting merges eluent, concentrate the Herba Desmodii Styracifolii total flavones.
Low-carbon alcohols in the described step 1) can be in methanol, ethanol, the isopropyl alcohol a kind of, consumption is 12～18 times of amounts of medical material.
Described step 2) the ultrafilter membrane aperture in is 5～10nm, and seeing through pressure is 0.3～0.5MPa.
The absorption flow speed control of hyperfiltration treatment liquid is 5～10ml/min in the described step 3).
Water lotion consumption in the described step 3) is 1～3BV, and ethanol liquid eluting is the 4-7BV65-80% alcoholic solution.
Advantage of the present invention is:
1) adopts concentrated dealcoholysis postprecipitation to remove water-insoluble impurity, remove water-soluble macromolecule impurity through ultrafilter membrane again, handle, alleviated the interference of impurity, strengthened the treating capacity of resin, the needs that the adaptation scale is handled resin through these remove impurity;
2) adopt low pure upper prop, reduced the adsorbance of macroporous resin, strengthened the treating capacity of macroporous resin impurity.
Further specify the present invention below in conjunction with the specific embodiment, but the scope of protection of present invention is not limited to following embodiment.
The specific embodiment:
Embodiment 1:
1) depletion money medical herbs material 1kg pulverizes, and is added to extract in the still, adopts the 12L50% methanol eddy to extract, and extracting solution places the vacuum concentration still, is concentrated into 1/2 of original volume, leaves standstill, and isolates supernatant.
2) with above-mentioned supernatant thin up, to cross ultrafilter membrane and carry out ultrafiltration, the ultrafilter membrane aperture is 5nm, seeing through pressure is that 0.5MPa removal water-soluble macromolecule gets hyperfiltration treatment liquid.
3) get AB-8 type macroporous resin wet method dress post, after the washing balance, above-mentioned hyperfiltration treatment liquid is slowly fed resin column, control absorption flow velocity is 5ml/min, uses the 3BV water elution earlier, uses 4BV80% alcoholic solution eluting more respectively, merge eluent, concentrate Herba Desmodii Styracifolii total flavones 8.5g.
Embodiment 2:
1) depletion money medical herbs material 1kg pulverizes, and is added to extract in the still, adopts the 18L70% alcohol reflux, and extracting solution places the vacuum concentration still, is concentrated into 2/3 of original volume, leaves standstill, and isolates supernatant.
2) with above-mentioned supernatant thin up, to cross ultrafilter membrane and carry out ultrafiltration, the ultrafilter membrane aperture is 10nm, seeing through pressure is that 0.3MPa removal water-soluble macromolecule gets hyperfiltration treatment liquid.
3) get D001 type macroporous resin wet method dress post, after the washing balance, above-mentioned hyperfiltration treatment liquid is slowly fed resin column, control absorption flow velocity is 6ml/min, uses the 1BV water elution earlier, uses 5BV75% alcoholic solution eluting more respectively, merge eluent, concentrate Herba Desmodii Styracifolii total flavones 9.1g.
Embodiment 3:
1) depletion money medical herbs material 5kg pulverizes, and is added to extract in the still, adopts 75L60% isopropyl alcohol reflux, extract,, and extracting solution places the vacuum concentration still, is concentrated into 2/3 of original volume, leaves standstill, and isolates supernatant.
2) with above-mentioned supernatant thin up, to cross ultrafilter membrane and carry out ultrafiltration, the ultrafilter membrane aperture is 5nm, seeing through pressure is that 0.3MPa removal water-soluble macromolecule gets hyperfiltration treatment liquid.
3) get AB-8 type macroporous resin wet method dress post, after the washing balance, above-mentioned hyperfiltration treatment liquid is slowly fed resin column, control absorption flow velocity is 10ml/min, uses the 2BV water elution earlier, uses 7BV80% alcoholic solution eluting more respectively, merge eluent, concentrate Herba Desmodii Styracifolii total flavones 35.4g.
Embodiment 4:
1) depletion money medical herbs material 10kg pulverizes, and is added to extract in the still, adopts the 140L65% alcohol reflux, and extracting solution places the vacuum concentration still, is concentrated into 3/5 of original volume, leaves standstill, and isolates supernatant.
2) with above-mentioned supernatant thin up, to cross ultrafilter membrane and carry out ultrafiltration, the ultrafilter membrane aperture is 10nm, seeing through pressure is that 0.4MPa removal water-soluble macromolecule gets hyperfiltration treatment liquid.
3) get D001 type macroporous resin wet method dress post, after the washing balance, above-mentioned hyperfiltration treatment liquid is slowly fed resin column, control absorption flow velocity is 8ml/min, uses the 2BV water elution earlier, uses 6BV75% alcoholic solution eluting more respectively, merge eluent, concentrate Herba Desmodii Styracifolii total flavones 77.1g.
Claims (4)
1. method of extracting total flavones from Herba Desmodii Styracifolii is characterized in that the method includes the steps of:
1) with the Herba Lysimachiae pulverizing medicinal materials, be added to and extract in the still, adopt 50～70% low-carbon alcohols reflux, extract,, extracting solution places the vacuum concentration still, is concentrated into 1/2～2/3 of former extracting liquid volume, leaves standstill, and isolates supernatant;
2) with above-mentioned supernatant thin up, cross ultrafilter membrane and carry out ultrafiltration, remove water-soluble macromolecule and get hyperfiltration treatment liquid.
3) get macroporous resin wet method dress post, above-mentioned hyperfiltration treatment liquid slowly fed resin column, first water eluting, reuse ethanol liquid eluting merges eluent, concentrate the Herba Desmodii Styracifolii total flavones.
2. a kind of method of extracting total flavones from Herba Desmodii Styracifolii as claimed in claim 1 is characterized in that described step 2) in the ultrafilter membrane aperture be 5～10nm.
3. a kind of method of extracting total flavones from Herba Desmodii Styracifolii as claimed in claim 1, the absorption flow speed control that it is characterized in that hyperfiltration treatment liquid in the described step 3) is 5～10ml/min.
4. a kind of method of extracting total flavones from Herba Desmodii Styracifolii as claimed in claim 1 is characterized in that the ethanol liquid eluting in the described step 3) is the 65-80% alcoholic solution.
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| CN103893258A (en) * | 2013-12-05 | 2014-07-02 | 人福医药集团股份公司 | Oral solid preparation containing desmodium styracifolium general flavone and application thereof |
| CN103893246A (en) * | 2013-12-05 | 2014-07-02 | 人福医药集团股份公司 | General flavanone capsule of desmodium styracifolium and preparation method and application thereof |
| CN103893247A (en) * | 2013-12-05 | 2014-07-02 | 人福医药集团股份公司 | Pharmaceutical composition as well as preparation method and application thereof |
| CN104492393A (en) * | 2014-11-13 | 2015-04-08 | 程金生 | Method for separating flavonoid substance in camellia nitidissima based on magnetic nanoparticles-PAMAM nano composite material |
| CN105212225A (en) * | 2015-04-24 | 2016-01-06 | 北京工业大学 | A kind of rosemary Halth-care composition being applied to cardiovascular and cerebrovascular disease |
| CN107677745A (en) * | 2017-09-29 | 2018-02-09 | 广西壮族自治区中医药研究院 | The quality determining method of Desmodium styracifolium extractive of general flavone |
| WO2018032611A1 (en) * | 2016-08-16 | 2018-02-22 | 南方科技大学 | Neuroprotective agent, and method for treating brain disease or disorder |
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- 2011-05-06 CN CN2011101178686A patent/CN102232993A/en active Pending
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| JP2016539173A (en) * | 2013-12-05 | 2016-12-15 | ウーハン オプティクス バリー ヒューマンウェル バイオ−ファーマシューティカル カンパニー リミテッド | Oral solid preparations containing broad-kind grasses and total flavonoids, and uses thereof |
| JP2016539955A (en) * | 2013-12-05 | 2016-12-22 | ヒューマンウェル ヘルスケア （グループ） カンパニー リミテッド | Drug composition, method for producing the same, and use |
| CN103893247A (en) * | 2013-12-05 | 2014-07-02 | 人福医药集团股份公司 | Pharmaceutical composition as well as preparation method and application thereof |
| CN103893258B (en) * | 2013-12-05 | 2017-09-29 | 人福医药集团股份公司 | Oral solid formulation and its application containing Desmodium styracifolium general flavone |
| WO2015081702A1 (en) * | 2013-12-05 | 2015-06-11 | 人福医药集团股份公司 | Drug combination, method of preparing same, and use thereof |
| WO2015081701A1 (en) * | 2013-12-05 | 2015-06-11 | 人福医药集团股份公司 | Desmodium styracifolium (osb.) merr. flavonoids capsule, method of preparing same, and application thereof |
| CN103893246A (en) * | 2013-12-05 | 2014-07-02 | 人福医药集团股份公司 | General flavanone capsule of desmodium styracifolium and preparation method and application thereof |
| JP2016540833A (en) * | 2013-12-05 | 2016-12-28 | 武漢光谷人福生物医薬有限公司Ｗｕｈａｎ Ｏｐｔｉｃｓ Ｖａｌｌｅｙ Ｈｕｍａｎｗｅｌｌ Ｂｉｏ−Ｐｈａｒｍａｃｅｕｔｉｃａｌ Ｃｏ． Ｌｔｄ． | Broad money sensation total flavonoid capsule, its production method and its application |
| WO2015081703A1 (en) * | 2013-12-05 | 2015-06-11 | 人福医药集团股份公司 | Solid dispersion containing desmodium styracifolium (osb.) merr. flavonoids, method of preparing same, and use thereof |
| CN103893258A (en) * | 2013-12-05 | 2014-07-02 | 人福医药集团股份公司 | Oral solid preparation containing desmodium styracifolium general flavone and application thereof |
| CN104492393B (en) * | 2014-11-13 | 2016-11-09 | 程金生 | Flavonoid substances separation method in Camellia nitidissima Chi based on magnetic nano-particle-PAMAM nano composite material |
| CN104492393A (en) * | 2014-11-13 | 2015-04-08 | 程金生 | Method for separating flavonoid substance in camellia nitidissima based on magnetic nanoparticles-PAMAM nano composite material |
| CN105212225A (en) * | 2015-04-24 | 2016-01-06 | 北京工业大学 | A kind of rosemary Halth-care composition being applied to cardiovascular and cerebrovascular disease |
| WO2018032611A1 (en) * | 2016-08-16 | 2018-02-22 | 南方科技大学 | Neuroprotective agent, and method for treating brain disease or disorder |
| CN107677745A (en) * | 2017-09-29 | 2018-02-09 | 广西壮族自治区中医药研究院 | The quality determining method of Desmodium styracifolium extractive of general flavone |
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Application publication date: 20111109 |