CN101234133A - Technique for using tribulus whole grass to extract total saponins of tribulus - Google Patents
Technique for using tribulus whole grass to extract total saponins of tribulus Download PDFInfo
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- CN101234133A CN101234133A CNA200710019035XA CN200710019035A CN101234133A CN 101234133 A CN101234133 A CN 101234133A CN A200710019035X A CNA200710019035X A CN A200710019035XA CN 200710019035 A CN200710019035 A CN 200710019035A CN 101234133 A CN101234133 A CN 101234133A
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Abstract
The invention relates to a field of plant extracting technology, in particular to a technique for extracting total saponins of tribulus from herba tribuli, which provides a technique for extracting total saponins of tribulus from herba tribuli, in order to solve the problems in the prior art that the raw material resources are limited and that the content of total saponins is low. The technique comprises the following steps in turn: (I) cutting the herba tribuli into short segments (0.5-1cm) and then alcohol extracting and concentrating, placing the concentrated solution in a low temperature of 4 DEG C or so for 12 to 48 hours, filtrating; (II) adding water into the filtrate until each 1ml contains 0.5g original medicinal material, passing a well treated nonpolar macroporous adsorbing resin with a velocity of flow of 2-5BV/h to absorb for 2-3 times, eluting with water until the effluent is of no color; (III) then eluting with 10-30 percent of ethanol until the effluent is of no color, concentrating and drying. Through the modern research, a preparation is finally acquired through extracting and purifying with herba tribuli as raw material. Compared with the traditional drug intake behavior, the technique has wide medicinal material resources, which in deed realizes the principle of changing waste into valuables.
Description
Affiliated technical field:
The present invention relates to technical field of plant extraction, be specifically related to a kind of technology of utilizing tribulus whole grass to extract total saponins of tribulus.
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.Medicinal part commonly used in the Chinese medicine Fructus Tribuli is its fruit, and its extract comprises compositions such as Fructus Tribuli steroidal saponin, flavone, polysaccharide and alkaloid.The total saponins that extracts in the Fructus Tribuli fruit (content about about 40%) is mainly used in the treatment cardiovascular and cerebrovascular disease clinically, as present Xinnaotong capsule for treating blood vessel of heart and brain or Xinnao Shutong sheet etc.The total saponins that extracts from Fructus Tribuli mainly comprises spirostanol saponin (spirostanol) and furostanol (furostanol) two classes, and the spiral shell sterol content is higher, and polarity is little, easily crystallization, and its chemical compound is mainly used in antifungal application; The furan sterol content 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.
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.But find in the research that because of comprising more ester soluble components such as chlorophyll in the puncturevine herb, therefore the content of total saponins is lower in its extract.
Summary of the invention:
The present invention will provide a kind of technology of utilizing tribulus whole grass to extract total saponins of tribulus, to overcome the lower problem of content of the raw material resources finite sum total saponins that prior art exists.
For overcoming the problem that prior art exists, the invention provides a kind of technology of utilizing tribulus whole grass to extract total saponins of tribulus, comprise the steps: successively
(1) get puncturevine herb, be cut into short section (0.5～1cm), alcohol extraction, concentrate, concentrated solution low temperature (about 4 ℃) left standstill 12～48 hours, filtered;
(2) filtrate adds water to every 1ml and contains crude drug 0.5g, and by the nonpolar macroporous adsorption resin absorption handled well 2～3 times, it is colourless that water is eluted to effluent with 2～5BV/h flow velocity;
(3) reuse 10～30% ethanol elutions are to colourless, be eluted to 2～5BV/h flow velocity with 4～7BV60～90% ethanol then colourless, collection 60～90% ethanol elution.(0.085Mpa) being evaporated to relative density is 1.25～1.30 extractum (25 ℃ of surveys), and (0.085Mpa) to do pulverize, cross 100 mesh sieves, promptly get of the present invention extract in 60 ℃ by drying under reduced pressure for extractum in 50 ℃.
In the above-mentioned steps (): add 5～10 times of amount 50～90% alcohol reflux 2～5 times during alcohol extraction, each 1～3 hour, filter, filtrate merges, and (0.085Mpa) is evaporated to nothing alcohol flavor at 40～60 ℃.
The resin that above-mentioned steps (two) is adopted is AB-8.Effect is better.
The resin that above-mentioned steps (two) is adopted can also be the nonpolar macroporous adsorption resin of D101 macroporous adsorbent resin or HPD series.
By modern study, we adopt puncturevine herb is that raw material is through extracting purification and it finally being made preparation.Compare with traditional medication custom, its crude drug source is wider, and really having accomplished turns waste into wealth.In extraction process, increased the stand at low temperature step especially, this step can effectively be removed ester soluble components such as chlorophyll, and the content of total saponins is higher in the extract.And this method is simple to operation, can satisfy industrial production requirement.
The specific embodiment:
Embodiment 1: a kind of technology of utilizing tribulus whole grass to extract total saponins of tribulus comprises the steps: successively
(1) get puncturevine herb, be cut into short section (0.5～1cm), add 8 times of amount 70% alcohol reflux 3 times, each 3 hours, filter, filtrate merges, (0.085Mpa) be evaporated to and do not have the alcohol flavor, concentrated solution low temperature (about 4 ℃) left standstill 48 hours, filtered at 50 ℃;
(2) filtrate adds water to every 1ml and contains crude drug 0.5g, and by the non polarity A B-8 absorption with macroporous adsorbent resin handled well 3 times, it is colourless that water is eluted to effluent with 2～5BV/h flow velocity.
(3) reuse 20% ethanol elution is to colourless, is eluted to colourlessly then with 2～5BV/h flow velocity with 5BV70% ethanol, collects 70% ethanol elution.(0.085Mpa) being evaporated to relative density is 1.25～1.30 extractum (50 ℃ of surveys), and (0.085Mpa) to do pulverize, cross 100 mesh sieves, promptly get of the present invention extract in 60 ℃ by drying under reduced pressure for extractum in 50 ℃.
Embodiment 2: a kind of technology of utilizing tribulus whole grass to extract total saponins of tribulus comprises the steps: successively
(1) get puncturevine herb, be cut into short section (0.5～1cm), add 5 times of amount 90% alcohol reflux 2 times, each 3 hours, filter, filtrate merges, (0.085Mpa) be evaporated to and do not have the alcohol flavor, concentrated solution low temperature (about 4 ℃) left standstill 36 hours, filtered at 40 ℃;
(2) filtrate adds water to every 1ml and contains crude drug 0.5g, and by the nonpolar D101 absorption with macroporous adsorbent resin handled well 2 times, it is colourless that water is eluted to effluent with 2～5BV/h flow velocity;
(3) reuse 30% ethanol elution is to colourless, is eluted to colourlessly then with 2～5BV/h flow velocity with 4BV90% ethanol, collects 60% ethanol elution.(0.085Mpa) being evaporated to relative density is 1.25～1.30 extractum (25 ℃ of surveys), and (0.085Mpa) to do pulverize, cross 100 mesh sieves, promptly get of the present invention extract in 60 ℃ by drying under reduced pressure for extractum in 50 ℃.
Embodiment 3: a kind of technology of utilizing tribulus whole grass to extract total saponins of tribulus comprises the steps: successively
(1) get puncturevine herb, be cut into short section (0.5～1cm), add 10 times of amount 50% alcohol reflux 5 times, each 1 hour, filter, filtrate merges, (0.085Mpa) be evaporated to and do not have the alcohol flavor, concentrated solution low temperature (about 4 ℃) left standstill 12 hours, filtered at 60 ℃;
(2) filtrate adds water to every 1ml and contains crude drug 0.5g, and by the HPD100 absorption with macroporous adsorbent resin handled well 3 times, it is colourless that water is eluted to effluent with 2～5BY/h flow velocity;
(3) reuse 10% ethanol elution is to colourless, is eluted to colourlessly then with 2～5BV/h flow velocity with 7BV60% ethanol, collects 90% ethanol elution.(0.085Mpa) being evaporated to relative density is 1.25～1.30 extractum (25 ℃ of surveys), and (0.085Mpa) to do pulverize, cross 100 mesh sieves, promptly get of the present invention extract in 60 ℃ by drying under reduced pressure for extractum in 50 ℃.
With removing chlorophyllous sample in the step (), compare with spissated sample after the alcohol extraction, measurement result sees the following form:
The resulting sample of embodiment is measured by the method on the ministry standard of health ministry, and the content of total saponins reaches more than 80%.
Claims (4)
1, the invention provides a kind of technology of utilizing tribulus whole grass to extract total saponins of tribulus, comprise the steps: successively
(1) get puncturevine herb, be cut into short section (0.5～1cm), alcohol extraction, concentrate, concentrated solution low temperature (about 4 ℃) left standstill 12～48 hours, filtered;
(2) filtrate adds water to every 1ml and contains crude drug 0.5g, and by the nonpolar macroporous adsorption resin absorption handled well 2～3 times, it is colourless that water is eluted to effluent with 2～5BV/h flow velocity;
(3) reuse 10～30% ethanol elutions are to colourless, be eluted to 2～5BV/h flow velocity with 4～7BV60～90% ethanol then colourless, collection 60～90% ethanol elution.(0.085Mpa) being evaporated to relative density is 1.25～1.30 extractum (25 ℃ of surveys), and (0.085Mpa) to do pulverize, cross 100 mesh sieves, promptly get of the present invention extract in 60 ℃ by drying under reduced pressure for extractum in 50 ℃.
2, a kind of technology of utilizing tribulus whole grass to extract total saponins of tribulus as claimed in claim 1, it is characterized in that: in the described step (): add 5～10 times of amount 50～90% alcohol reflux 2～5 times during alcohol extraction, each 1～3 hour, filter, filtrate merges, and (0.085Mpa) is evaporated to nothing alcohol flavor at 40～60 ℃.
3, a kind of technology of utilizing tribulus whole grass to extract total saponins of tribulus as claimed in claim 1 or 2, it is characterized in that: the resin that described step (two) is adopted is AB-8.
4, a kind of technology of utilizing tribulus whole grass to extract total saponins of tribulus as claimed in claim 1 or 2 is characterized in that: the resin that described step (two) is adopted can also be the nonpolar macroporous adsorption resin of D101 macroporous adsorbent resin or HPD series.
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| CNB200710019035XA CN100496529C (en) | 2007-11-09 | 2007-11-09 | Technique for using tribulus whole grass to extract total saponins of tribulus |
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| CNB200710019035XA CN100496529C (en) | 2007-11-09 | 2007-11-09 | Technique for using tribulus whole grass to extract total saponins of tribulus |
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| CN101234133A true CN101234133A (en) | 2008-08-06 |
| CN100496529C CN100496529C (en) | 2009-06-10 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610397A (en) * | 2015-01-22 | 2015-05-13 | 湖南杰萃生物技术有限公司 | Method for extracting protodioscin from stems and leaves of tribulus terrestris |
| CN105311067A (en) * | 2014-07-29 | 2016-02-10 | 西安旭煌生物技术有限公司 | Method for extracting total tribulus terrestris saponins from stems and leaves of tribulus terrestris |
| CN109180774A (en) * | 2018-09-03 | 2019-01-11 | 长白山制药股份有限公司 | A kind of pharmaceutical composition and preparation method thereof containing Fructus Tribuli fruit total saponin |
| CN113134020A (en) * | 2021-05-14 | 2021-07-20 | 内蒙古民族大学 | Preparation method and application of Mongolian medicine tribulus terrestris ethanol extract |
-
2007
- 2007-11-09 CN CNB200710019035XA patent/CN100496529C/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105311067A (en) * | 2014-07-29 | 2016-02-10 | 西安旭煌生物技术有限公司 | Method for extracting total tribulus terrestris saponins from stems and leaves of tribulus terrestris |
| CN104610397A (en) * | 2015-01-22 | 2015-05-13 | 湖南杰萃生物技术有限公司 | Method for extracting protodioscin from stems and leaves of tribulus terrestris |
| CN109180774A (en) * | 2018-09-03 | 2019-01-11 | 长白山制药股份有限公司 | A kind of pharmaceutical composition and preparation method thereof containing Fructus Tribuli fruit total saponin |
| CN113134020A (en) * | 2021-05-14 | 2021-07-20 | 内蒙古民族大学 | Preparation method and application of Mongolian medicine tribulus terrestris ethanol extract |
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| CN100496529C (en) | 2009-06-10 |
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