CN102824520A - Preparation method of common diuranthera root saponin - Google Patents
Preparation method of common diuranthera root saponin Download PDFInfo
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- CN102824520A CN102824520A CN 201210373267 CN201210373267A CN102824520A CN 102824520 A CN102824520 A CN 102824520A CN 201210373267 CN201210373267 CN 201210373267 CN 201210373267 A CN201210373267 A CN 201210373267A CN 102824520 A CN102824520 A CN 102824520A
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- ethanol
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- radix diurantherae
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Abstract
The invention discloses a preparation method of common diuranthera root saponin. The method is technically characterized by comprising the following steps of: grinding the common diuranthera root and extracting with supercritical CO2; performing ultrasonic extraction on the extract with 60-95% ethanol; performing reduced-pressure concentration on the extract solution; adsorbing with a macroporous adsorption resin column; adding kieselguhr active carbon mixture into the eluent and heating and stirring; filtering while the product is hot; and performing reduced-pressure concentration and spray drying to obtain the common diuranthera root saponin. The preparation method disclosed by the invention has stable technology and high extraction rate, ensures safe production and prevents pollution in the operation process.
Description
Technical field
The invention belongs to the extracted form natural plant separation field, relate to a kind of method for preparing of Radix diurantherae majoris saponin.
Background technology
Radix diurantherae majoris is a Liliaceae little egret grass platymiscium little egret grass
Diuranthera majorHemsl. root has another name called Herba Allii bulleyani (" choosing of Yunnan Chinese herbal medicine "), Silene tatarinowii Regel-Melandrium tatarinwiii (Regel) Tsui. (" national Chinese herbal medicine compilation ").Be distributed in Sichuan, Guizhou, Yunnan.Radix diurantherae majoris is sweet, and is flat, has antiinflammatory, hemostatic effect, cures mainly traumatic hemorrhage.Mainly contain the terpene glycosides in the root: Radix diurantherae majoris glycosides (Diuranthoside) A, B, C are promptly new for high sapogenin 3-O-β-D-glucopyranosyl (1 → 2)-[β-D-xylopyranosyl (1 → 3)]-β-D-glucopyranosyl (1 → 4)-β-D-galactopyranoside; New hecogenin 3-O-β-D-glucopyranosyl (1 → 3)-β-D-xylopyranosyl (1 → 3)-[β-D-glucopyranosyl (1 → 2)]-β-D-glucopyranosyl (1 → 4)-β-D-galactopyranoside and new hecogenin 3-O-β-D-glucopyranosyl (1 → 3)-β-D-glucopyranosyl (1 → 2)-[β-D-glucopyranosyl (1 → 3)-β-D-xylopyranosyl (1 → 3)]-β-D-glucopyranosyl (1 → 4)-β-D-galactopyranoside, and asparagus filicicum Ham glycosides.
Steroidal saponin is a kind of native compound that occurring in nature extensively distributes; Research in recent years shows; Steroidal saponin has pharmacological action widely and important biological, like antitumor, antifungal, prevent and treat cardiovascular disease, blood sugar lowering, immunomodulating etc., has caused global concern.The present invention provides a kind of method for preparing of Radix diurantherae majoris saponin, can further enrich steroidal saponin medication resource better.
Through retrieval, still do not have at present and extract the method report for preparing the Radix diurantherae majoris saponin.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing of Radix diurantherae majoris saponin.The inventive method prepares the Radix diurantherae majoris saponin, and method is simple, and is energy-conservation, is easy to control.
The objective of the invention is to adopt following technical scheme to realize:
A kind of method for preparing of Radix diurantherae majoris saponin is characterized in that: Radix diurantherae majoris is pulverized, added entrainer, through supercritical CO
2Extraction, extraction conditions is: extracting pressure 23-37.5MPa, extraction temperature 40-60 ℃; Extraction time 3.5-5.5h, the gained extract is used the 60-95% ethanol ultrasonic extraction, and extracting solution is evaporated to small size; Disperse with hot water, through macroporous adsorptive resins absorption, eluent adds kieselguhr Mixture of Activated Carbon heated and stirred again; Filtered while hot, concentrating under reduced pressure, spray drying promptly gets the Radix diurantherae majoris saponin.
Said entrainer is ethanol, the n-butyl alcohol mixed solution that is added with sodium lauryl sulphate; The concentration of sodium lauryl sulphate is 0.02-0.05mol/L; Ethanol, n-butyl alcohol volume ratio are 4:1-1:1, and ethanol is the ethanol water of 70-85%, and the entrainer addition is the 2-4ml/g crude drug.
Said macroporous adsorbent resin is selected a kind of among XAD761, HPD400, HZ801 or the HP50 for use, and eluant is the 60%-80% alcoholic solution of 3-5BV.
The invention has the advantages that: the mixed solution of surfactant and polyhydric alcohol has improved supercritical CO as entrainer
2Extraction yield has good selectivity simultaneously, can obtain the Radix diurantherae majoris saponin extract of higher degree; The inventive method have technology simple, be easy to advantages such as control, the high and low power consumption of product purity.
The specific embodiment:
Embodiment 1:
Take by weighing the 5kg Radix diurantherae majoris and put into extractor, preparation contains ethanol n-butyl alcohol mixed solution (85% ethanol: n-butyl alcohol=3:1) as entrainer, add 14L in extractor, at extracting pressure 23.3MPa of 0.03mol/L sodium lauryl sulphate; Dynamic extraction 4h under 45 ℃ of conditions of extraction temperature collects the extract of from separator, emitting, and with 70% ethanol ultrasonic extraction 45min, extracting solution is evaporated to small size; Adsorb through the HP50 macroporous adsorptive resins after adding aqueous dispersion, it is closely colourless that first water is eluted to water lotion, discards eluent; 70% ethanol elution of 4 times of column volumes of reuse is collected eluent, and eluent is again through the magnesium oxide post; Collect fluid injection down, concentrating under reduced pressure reclaims ethanol; Lyophilization, pulverizing obtain white powder, and wherein the Radix diurantherae majoris total saponin content 89%.
Embodiment 2:
Take by weighing the 5kg Radix diurantherae majoris and put into extractor, preparation contains ethanol n-butyl alcohol mixed solution (80% ethanol: n-butyl alcohol=1:1) as entrainer, add 10L in extractor, at extracting pressure 26.7MPa of 0.04mol/L sodium lauryl sulphate; Dynamic extraction 4h under 40 ℃ of conditions of extraction temperature collects the extract of from separator, emitting, and with 30% ethanol ultrasonic extraction 60min, extracting solution is evaporated to small size; Adsorb through the XAD761 macroporous adsorptive resins after adding aqueous dispersion, it is closely colourless that first water is eluted to water lotion, discards eluent; 65% ethanol elution of 3 times of column volumes of reuse is collected eluent, and eluent is again through the magnesium oxide post; Collect fluid injection down, concentrating under reduced pressure reclaims ethanol; Lyophilization, pulverizing obtain white powder, and wherein the Radix diurantherae majoris total saponin content 84%.
Embodiment 3:
Take by weighing the 5kg Radix diurantherae majoris and put into extractor, preparation contains ethanol n-butyl alcohol mixed solution (70% ethanol: n-butyl alcohol=2:1) as entrainer, add 18L in extractor, at extracting pressure 30.8MPa of 0.05mol/L sodium lauryl sulphate; Dynamic extraction 3.5h under 47 ℃ of conditions of extraction temperature collects the extract of from separator, emitting, and with 80% ethanol ultrasonic extraction 50min, extracting solution is evaporated to small size; Adsorb through the HPD400 macroporous adsorptive resins after adding aqueous dispersion, it is closely colourless that first water is eluted to water lotion, discards eluent; 80% ethanol elution of 5 times of column volumes of reuse is collected eluent, and eluent is again through the magnesium oxide post; Collect fluid injection down, concentrating under reduced pressure reclaims ethanol; Lyophilization, pulverizing obtain white powder, and wherein the Radix diurantherae majoris total saponin content 88%.
Embodiment 4:
Take by weighing the 10kg Radix diurantherae majoris and put into extractor, preparation contains ethanol n-butyl alcohol mixed solution (75% ethanol: n-butyl alcohol=3:1) as entrainer, add 20L in extractor, at extracting pressure 37.5MPa of 0.02mol/L sodium lauryl sulphate; Dynamic extraction 5.5h under 60 ℃ of conditions of extraction temperature collects the extract of from separator, emitting, and with 95% ethanol ultrasonic extraction 30min, extracting solution is evaporated to small size; Adsorb through the HZ801 macroporous adsorptive resins after adding aqueous dispersion, it is closely colourless that first water is eluted to water lotion, discards eluent; 75% ethanol elution of 4 times of column volumes of reuse is collected eluent, and eluent is again through the magnesium oxide post; Collect fluid injection down, concentrating under reduced pressure reclaims ethanol; Lyophilization, pulverizing obtain white powder, and wherein the Radix diurantherae majoris total saponin content 82%.
Embodiment 5:
Take by weighing the 10kg Radix diurantherae majoris and put into extractor, preparation contains ethanol n-butyl alcohol mixed solution (80% ethanol: n-butyl alcohol=4:1) as entrainer, add 12L in extractor, at extracting pressure 34.1MPa of 0.04mol/L sodium lauryl sulphate; Dynamic extraction 4.5h under 54 ℃ of conditions of extraction temperature collects the extract of from separator, emitting, and with 60% ethanol ultrasonic extraction 55min, extracting solution is evaporated to small size; Adsorb through the HP50 macroporous adsorptive resins after adding aqueous dispersion, it is closely colourless that first water is eluted to water lotion, discards eluent; 70% ethanol elution of 5 times of column volumes of reuse is collected eluent, and eluent is again through the magnesium oxide post; Collect fluid injection down, concentrating under reduced pressure reclaims ethanol; Lyophilization, pulverizing obtain white powder, and wherein the Radix diurantherae majoris total saponin content 86%.
Claims (3)
1. the method for preparing of a Radix diurantherae majoris saponin is characterized in that: Radix diurantherae majoris is pulverized, added entrainer, through supercritical CO
2Extraction, extraction conditions is: extracting pressure 23-37.5MPa, extraction temperature 40-60 ℃; Extraction time 3.5-5.5h, the gained extract is used the 60-95% ethanol ultrasonic extraction, and extracting solution is evaporated to small size; Disperse with hot water, through macroporous adsorptive resins absorption, eluent adds kieselguhr Mixture of Activated Carbon heated and stirred again; Filtered while hot, concentrating under reduced pressure, spray drying promptly gets the Radix diurantherae majoris saponin.
2. the method for claim 1; It is characterized in that said entrainer is ethanol, the n-butyl alcohol mixed solution that is added with sodium lauryl sulphate; The concentration of sodium lauryl sulphate is 0.02-0.05mol/L; Ethanol, n-butyl alcohol volume ratio are 4:1-1:1, and ethanol is the ethanol water of 70-85%, and the entrainer addition is the 2-4ml/g crude drug.
3. the method for claim 1 is characterized in that said macroporous adsorbent resin selects a kind of among XAD761, HPD400, HZ801 or the HP50 for use, and eluant is the 60%-80% alcoholic solution of 3-5BV.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201210373267 CN102824520A (en) | 2012-09-27 | 2012-09-27 | Preparation method of common diuranthera root saponin |
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| CN 201210373267 CN102824520A (en) | 2012-09-27 | 2012-09-27 | Preparation method of common diuranthera root saponin |
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Application publication date: 20121219 |