CN101455696B - Puncturevine herb extract rich in furostanol saponin and preparation method thereof - Google Patents
Puncturevine herb extract rich in furostanol saponin and preparation method thereof Download PDFInfo
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- CN101455696B CN101455696B CN2007101885905A CN200710188590A CN101455696B CN 101455696 B CN101455696 B CN 101455696B CN 2007101885905 A CN2007101885905 A CN 2007101885905A CN 200710188590 A CN200710188590 A CN 200710188590A CN 101455696 B CN101455696 B CN 101455696B
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Abstract
The invention relates to the technical field of raw material drug extracted from plants, concretely to a caltrop herb extract and a preparation method thereof. The invention provides a caltrop herb extract containing rich furan steroid saponin and a preparation method thereof to solve the problem of low content of furan steroid saponin in extracts existing in the prior art. The caltrop herb extract containing rich furan steroid saponin is prepared by the following method comprising the following steps: 1, cutting caltrop herbs into short sections, adding water to decoct, extracting under reflux and filtering for the first time; adding water to decoct, extracting under reflux and filtering for the second time; adding water to decoct, extracting under reflux and filtering for the third time, combining the filtrate; 2, adding in ethanol, standing, filtering, concentrating the filtrate by lowering pressure until no alcohol smell is left; 3, passing through treated polymeric adsorbent, washing with water until effluent is colourless; 4, concentrating ethanol eluent by lowering pressure into extract, drying the extract by lowering pressure, crushing, screening, thus forming the product of the invention.
Description
Technical field:
The present invention relates to the plant extract technical field of raw material drug, be specifically related to a kind of puncturevine herb extract and preparation method thereof.
Technical background:
Fructus Tribuli has another name called Fructus Atriplicis Sibiricae, Fructus Tribuli, hard Fructus Tribuli.Nature and flavor suffering, hardship, tepor, slightly poisonous, go into liver, lung meridian, have diffusing wind, make eye bright, the effect of the therapeutic method to keep the adverse QI flowing downwards, promoting the circulation of blood, the kidney invigorating and essence nourishing.Chinese medicine Fructus Tribuli tradition medicinal part is its fruit, and it mainly contains compositions such as steroidal saponin, flavone, polysaccharide and alkaloid.The total saponins that extracts from Fructus Tribuli mainly comprises spirostanol saponin (spirostanol) and furostanol (furostanol) two classes, and spirostanol saponin content is higher, and polarity is little, easily crystallization, and its chemical compound is mainly used in antifungal application; Content of furostanol saponin is lower, and water solublity is bigger, is difficult for crystallization, through pharmacological testing and effect experiment proof resisting cardiovascular is had tangible prevention and therapeutical effect.Active component based on the puncturevine furostanol saponins compositions can be prepared into the treatment blood circulation promoting and blood stasis dispelling, promoting the circulation of QI to relieve pain, the medicine of the various dosage forms of the blood-stasis internal-depression disease of treatment coronary heart disease, angina pectoris.
Narrower because of Fructus Tribuli fruit source, and pluck, handle trouble, therefore the utilization to its herb becomes the problem that pharmaceuticals industry is paid close attention to.Adopt puncturevine herb to extract, crude drug source is extensive, and having accomplished turns waste into wealth, and has removed complicated harvesting operation from.But find in the research, because of comprising compositions such as more chlorophyll, Fructus Tribuli polysaccharide, volatile oil, fatty oil and part biological alkali in the puncturevine herb, also comprise a spot of flavone compound, content of furostanol saponin very low (content about about 10%) in the extract that adopts traditional handicraft to extract, it is undesirable to be applied in the preparation of resisting cardiovascular effect.
Summary of the invention:
The objective of the invention is to provide a kind of puncturevine herb extract that is rich in furostanol and preparation method thereof, to overcome the low problem of content of furostanol saponin in the extract that prior art exists.
A kind of puncturevine herb extract that is rich in furostanol, finished by following method preparation: this method comprises the steps: successively
One, get puncturevine herb, (0.5～1cm), the first fries in shallow oil that to add pH value be 4.5～6.0 water, and amount of water is 7～10 times, carries out reflux, extract,, each 1.5～3 hours, filters to be cut into short section; Second fries in shallow oil that to add pH value be 5.5～6.5 water, and amount of water is 5～7 times, carries out reflux, extract,, each 0.5～1.5 hour, filters; The 3rd fries in shallow oil that to add pH value be 7.5～8.5 water, and amount of water is 5～7 times, carries out reflux, extract,, and each 0.5～1.5 hour, filter, filtrate merges;
Two, merging filtrate, concentrating under reduced pressure adds ethanol and leaves standstill, and filters, and filtrate is evaporated to does not again have the alcohol flavor;
Three, filtrate adds water, and by nonpolar (or low pole) macroporous adsorbent resin of having handled well, it is colourless that water is eluted to effluent;
Four, reuse 10～30% ethanol elutions use 60～90% ethanol elutions to colourless to colourless then, collect 60～90% ethanol elution, and concentrating under reduced pressure is an extractum, and the extractum drying under reduced pressure is pulverized to doing, and sieves, and promptly gets thing of the present invention.
A kind of puncturevine herb extract that is rich in furostanol, finished by following method preparation: this method comprises the steps: successively
One, get puncturevine herb, (0.5～1cm), the first fries in shallow oil that to add pH value be 4.5～6.0 water, and amount of water is 7～10 times, carries out reflux, extract,, each 1.5～3 hours, filters to be cut into short section; Second fries in shallow oil that to add pH value be 5.5～6.5 water, and amount of water is 5～7 times, carries out reflux, extract,, each 0.5～1.5 hour, filters; The 3rd fries in shallow oil that to add pH value be 7.5～8.5 water, and amount of water is 5～7 times, carries out reflux, extract,, and each 0.5～1.5 hour, filter, filtrate merges;
Two, (0.085Mpa) be evaporated to relative density 1.05～1.15, add ethanol and make that to contain the alcohol amount be 55～75%, left standstill 12～24 hours, filter, filtrate (0.085Mpa) is evaporated to and does not have the alcohol flavor at 40～60 ℃ again at 40～60 ℃ with merging filtrate;
Three, filtrate adds water to every 1ml and contains crude drug 0.25g, and by nonpolar (or low pole) macroporous adsorbent resin of having handled well, it is colourless that water is eluted to effluent.
Four, reuse 10～30% ethanol elutions are to colourless, use 60～90% ethanol elutions to colourless then, collect 60～90% ethanol elution, in 50～60 ℃ of (0.085Mpa) concentrating under reduced pressure, to relative density be 1.25～1.30 extractum (50 ℃ of surveys), (0.085Mpa) to do pulverize in 50～70 ℃ by drying under reduced pressure for extractum, cross 80～120 mesh sieves, promptly get thing of the present invention.
The resin that above-mentioned steps three is adopted can be similar nonpolar macroporous adsorption resins such as AB-8, D101 macroporous adsorbent resin, HPD series.
By studying for a long period of time, we adopt puncturevine herb is that raw material extracts purification, improves the yield of effective site in this process by specific technology.Concrete advantage is described as follows:
One, raw material sources are extensive.Its crude drug source is wider, and plucks, handles easily, suitability for industrialized production preferably, and really having accomplished turns waste into wealth.
Two, the content of furostanol compounds higher (content 〉=50%), be crude drug purity height: as the treatment blood circulation promoting and blood stasis dispelling, promoting the circulation of QI to relieve pain, the crude drug of the blood-stasis internal-depression disease of coronary heart disease, angina pectoris, the content of furostanol compounds is directly connected to its therapeutic effect.In recent years, various countries are continuous to this plant research, but the extracted amount of furostanol compounds also can not seen as the research of target.The present invention has effectively improved the content of furostanol compounds on the preparation method, makes clinical efficacy more obvious.Its preparation method is a complete brand new technical scheme.Wherein more outstanding with following 2 performances especially:
(1), the present invention mainly considers to provide a kind of new semi-bionic extraction alcohol precipitation (being SBAE) method from the biopharmaceutics angle, and the Fructus Tribuli extract that extracts has been carried out effective purification, kept active component.This method is to imitate oral drugs at the gastrointestinal transport process, adopts the acid water of selected pH and alkaline water to extract continuously successively, its objective is to extract to contain index components high " active mixture ".The present invention adopts from biopharmaceutical angle simulation oral administration, and medicine is formulated through the principle of gastrointestinal tract transhipment, both considered monomer component, can consider " active blending constituent " again, can give full play to the comprehensive function characteristics of mix ingredients like this, help again controlling the quality of the pharmaceutical preparations with monomer component.Adopt the semi-bionic extraction alcohol deposition method, can remove chlorophyll, Fructus Tribuli polysaccharide, volatile oil, fatty oil and chemical compounds such as part biological alkali and flavonoid.Make extract preferably through gastrointestinal absorption.
(2), in second step of the present invention: precipitate with ethanol is mainly used to remove the part water-solubility impurity, finishes purification through the back macroporous adsorbent resin again.
Three, the method for preparing extract of the present invention mainly is to adopt semi-biomimetic method to extract, and preferably through gastrointestinal absorption, therefore prepared preparation also more helps the abundant absorption of human body, has improved the result of use of product, and clinical efficacy is more obvious.
The specific embodiment:
To be described in detail the present invention by specific embodiment below.
Embodiment 1, and a kind of puncturevine herb extract is finished by following method preparation, and said method comprises the steps: successively
One, get puncturevine herb, (0.5～1cm), the first fries in shallow oil that to add pH value be 5.0 water, and amount of water is 8 times, carries out reflux, extract,, each 2 hours, filters to be cut into short section; Second fries in shallow oil that to add pH value be 6.0 water, and amount of water is 6 times, carries out reflux, extract,, each 1 hour, filters; The 3rd fries in shallow oil that to add pH value be 8.0 water, and amount of water is 6 times, carries out reflux, extract,, and each 1 hour, filter, filtrate merges.
Two, (0.085Mpa) be evaporated to relative density 1.05～1.15, add ethanol and make that to contain the alcohol amount be 65%, left standstill 18 hours, filter, filtrate (0.085Mpa) is evaporated to and does not have the alcohol flavor at 50 ℃ again at 55 ℃ with merging filtrate.
Three, filtrate adds water to every 1ml and contains crude drug 0.25g, and by the AB-8 macroporous adsorbent resin of having handled well, it is colourless that water is eluted to effluent.
Four, reuse 30% ethanol elution is to colourless, use 90% ethanol elution to colourless then, collect 90% ethanol elution, in 50 ℃ of (0.085Mpa) concentrating under reduced pressure, to relative density be 1.25～1.30 extractum (50 ℃ of surveys), (0.085Mpa) to do pulverize in 60 ℃ by drying under reduced pressure for extractum, cross 100 mesh sieves, promptly get extract of the present invention.
Embodiment 2, and a kind of puncturevine herb extract is finished by following method preparation, and said method comprises the steps: successively
One, get puncturevine herb, (0.5～1cm), the first fries in shallow oil that to add pH value be 6.0 water, and amount of water is 10 times, carries out reflux, extract,, each 1.5 hours, filters to be cut into short section; Second fries in shallow oil that to add pH value be 6.5 water, and amount of water is 8 times, carries out reflux, extract,, each 1.5 hours, filters; The 3rd fries in shallow oil that to add pH value be 8.5 water, and amount of water is 8 times, carries out reflux, extract,, and each 0.5 hour, filter, filtrate merges.
Two, (0.085Mpa) be evaporated to relative density 1.05～1.15, add ethanol and make that to contain the alcohol amount be 75%, left standstill 12 hours, filter, filtrate (0.085Mpa) is evaporated to and does not have the alcohol flavor at 60 ℃ again at 40 ℃ with merging filtrate.
Three, filtrate adds water to every 1ml and contains crude drug 0.25g, and by the D101 macroporous adsorbent resin of having handled well, it is colourless that water is eluted to effluent.
Four, reuse 10% ethanol elution is to colourless, use 70% ethanol elution to colourless then, collect 70% ethanol elution, in 60 ℃ of (0.085Mpa) concentrating under reduced pressure, to relative density be 1.25～1.30 extractum (50 ℃ of surveys), (0.085Mpa) to do pulverize in 60 ℃ by drying under reduced pressure for extractum, cross 120 mesh sieves, promptly get thing of the present invention.
Embodiment 3, and a kind of puncturevine herb extract that is rich in furostanol is finished by following method preparation, and this method comprises the steps: successively
One, get puncturevine herb, (0.5～1cm), the first fries in shallow oil that to add pH value be 4.5 water, and amount of water is 7 times, carries out reflux, extract,, each 3 hours, filters to be cut into short section; Second fries in shallow oil that to add pH value be 5.5 water, and amount of water is 7 times, carries out reflux, extract,, each 0.5 hour, filters; The 3rd fries in shallow oil that to add pH value be 8.0 water, and amount of water is 7 times, carries out reflux, extract,, and each 1.5 hours, filter, filtrate merges.
Two, (0.085Mpa) be evaporated to relative density 1.05～1.15, add ethanol and make that to contain the alcohol amount be 60%, left standstill 24 hours, filter, filtrate (0.085Mpa) is evaporated to and does not have the alcohol flavor at 40 ℃ again at 60 ℃ with merging filtrate.
Three, filtrate adds water to every 1ml and contains crude drug 0.25g, and by the HPD macroporous adsorbent resin of having handled well, it is colourless that water is eluted to effluent.
Four, reuse 20% ethanol elution uses 60% ethanol elution to colourless to colourless then, collects 60% ethanol elution.In 55 ℃ (0.085Mpa) concentrating under reduced pressure, to relative density be 1.25～1.30 extractum (50 ℃ of surveys), (0.085Mpa) to do pulverize, cross 80 mesh sieves, promptly get of the present invention thing in 65 ℃ by drying under reduced pressure for extractum.
Claims (3)
1. puncturevine herb extract that is rich in furostanol, finished by following method preparation: this method comprises the steps: successively
1) get puncturevine herb, be cut into the short section of 0.5～1cm, first fries in shallow oil that to add pH value be 4.5～6.0 water, and amount of water is 7～10 times, carries out reflux, extract,, each 1.5～3 hours, filters; Second fries in shallow oil that to add pH value be 5.5～6.5 water, and amount of water is 5～7 times, carries out reflux, extract,, each 0.5～1.5 hour, filters; The 3rd fries in shallow oil that to add pH value be 7.5～8.5 water, and amount of water is 5～7 times, carries out reflux, extract,, and each 0.5～1.5 hour, filter, filtrate merges;
2) merging filtrate, concentrating under reduced pressure adds ethanol and leaves standstill, and filters, and filtrate is evaporated to does not again have the alcohol flavor;
3) filtrate adds water, and by the nonpolar macroporous adsorption resin of having handled well, it is colourless that water is eluted to effluent;
4) reuse 10～30% ethanol elutions use 60～90% ethanol elutions to colourless to colourless then, collect 60～90% ethanol elution, and concentrating under reduced pressure is an extractum, and the extractum drying under reduced pressure is pulverized to doing, and sieves, promptly.
2. a puncturevine herb extract that is rich in furostanol is finished by following method preparation, and it is characterized in that: this method comprises the steps: successively
1) get puncturevine herb, be cut into the short section of 0.5～1cm, first fries in shallow oil that to add pH value be 4.5～6.0 water, and amount of water is 7～10 times, carries out reflux, extract,, each 1.5～3 hours, filters; Second fries in shallow oil that to add pH value be 5.5～6.5 water, and amount of water is 5～7 times, carries out reflux, extract,, each 0.5～1.5 hour, filters; The 3rd fries in shallow oil that to add pH value be 7.5～8.5 water, and amount of water is 5～7 times, carries out reflux, extract,, and each 0.5～1.5 hour, filter, filtrate merges;
2) with merging filtrate 40～60 ℃ and-be evaporated to relative density 1.05～1.15 under the 0.085MPa, add ethanol and make that to contain the alcohol amount be 55～75%, left standstill 12～24 hours, filter, filtrate again 40～60 ℃ and-be evaporated under the 0.085MPa and do not have the alcohol flavor;
3) filtrate adds water to every 1ml and contains crude drug 0.25g, and by the nonpolar macroporous adsorption resin of having handled well, it is colourless that water is eluted to effluent;
4) reuse 10～30% ethanol elutions are to colourless, use 60～90% ethanol elutions to colourless then, collect 60～90% ethanol elution, in 50～60 ℃ and-0.085MPa under concentrating under reduced pressure, to survey relative density in the time of 50 ℃ is 1.25～1.30 extractum, extractum in 50～70 ℃ and-0.085MPa under drying under reduced pressure to doing, pulverize, cross 80～120 mesh sieves, promptly.
3. a kind of puncturevine herb extract that is rich in furostanol as claimed in claim 2 is characterized in that: the resin that described step 3) adopted is AB-8, D101 macroporous adsorbent resin, the HPD nonpolar macroporous adsorption resin.
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| CN2007101885905A CN101455696B (en) | 2007-12-12 | 2007-12-12 | Puncturevine herb extract rich in furostanol saponin and preparation method thereof |
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| CN2007101885905A CN101455696B (en) | 2007-12-12 | 2007-12-12 | Puncturevine herb extract rich in furostanol saponin and preparation method thereof |
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| CN101455696B true CN101455696B (en) | 2011-12-14 |
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| CN104352540B (en) * | 2014-10-20 | 2017-08-18 | 成都中医药大学 | It is a kind of to treat hydrogel matrix type sustained release tablets of coronary disease and angina pectoris and preparation method thereof |
| CN104610397B (en) * | 2015-01-22 | 2018-03-06 | 湖南杰萃生物技术有限公司 | A kind of method that Protodioscin is extracted in the cauline leaf from puncture vine |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1039595A (en) * | 1988-05-22 | 1990-02-14 | 洮南市第一制药厂 | The production technique of puncture vine total saponin |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1039595A (en) * | 1988-05-22 | 1990-02-14 | 洮南市第一制药厂 | The production technique of puncture vine total saponin |
Non-Patent Citations (2)
| Title |
|---|
| 李立等.半仿生法提取黄芩苷的研究.《中成药》.2007,第29卷(第10期),1527-1528. * |
| 王宇卿等.中药半仿生提取法的研究进展.《医药导报》.2007,第26卷(第7期),754-756. * |
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