CN102234307A - Method for extracting and separating pardifomoside from Lysimachia paridiformis - Google Patents
Method for extracting and separating pardifomoside from Lysimachia paridiformis Download PDFInfo
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- CN102234307A CN102234307A CN2011101178402A CN201110117840A CN102234307A CN 102234307 A CN102234307 A CN 102234307A CN 2011101178402 A CN2011101178402 A CN 2011101178402A CN 201110117840 A CN201110117840 A CN 201110117840A CN 102234307 A CN102234307 A CN 102234307A
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- paris polyphylla
- lysimachia sikokiana
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Abstract
The invention relates to a method for extracting and separating pardifomoside from Lysimachia paridiformis. The method comprises the following steps: crushing Lysimachia paridiformis, carrying out enzymolysis, adding 5-10 times the amount of 60-80% ethanol solution to ultrasonically extract for 2-3 times, adding activated carbon to the extract liquid for decolorizing, filtering, concentrating the filtrate to recover ethanol, adding the concentrated liquid to a polyamide column for chromatography, eluting with an alcohol aqueous solution, concentrating and drying the eluate to obtain a crude product, separating the crude product by high-speed countercurrent chromatography to obtain high-purity pardifomoside. The method provided by the invention has a stable process, and the obtained product has a high pardifomoside content (up to 98% or above).
Description
Technical field:
The invention belongs to the extractive technique field of crude substance, relate to a kind of from the Paris polyphylla Lysimachia sikokiana method of extraction separation Paris polyphylla Lysimachia sikokiana glycosides.
Background technology:
The Paris polyphylla Lysimachia sikokiana is the herb of Primulaceae Lysimachia plant Paris polyphylla Lysimachia sikokiana, has another name called four slices watts, red Herba Chloranthi Henryi (Herba Choranthi seu Lysimachiae), yunna spiraea, Parisshape loosestrife etc.Mainly be distributed in ground such as Hubei, Hunan, Sichuan, Guizhou.The Paris polyphylla Lysimachia sikokiana have dispel rheumatism, the effect of promoting blood circulation and stopping pain, cough-relieving, detoxifcation, cure mainly rheumatalgia, epigastric pain, cough, wound, furuncle and treat diseases such as sore, venomous snake bite.Among the people more than with herb decoction treatment rheumatic numbness, wound and postpartum hemorrhage, its electuary has excitation and anastalsis to the uterus.
The Paris polyphylla Lysimachia sikokiana contains Paris polyphylla Lysimachia sikokiana glycosides (paridiformoside) isoreactivity composition.What merit doubly waits by discovering that Paris polyphylla Lysimachia sikokiana glycosides the more plants the uterus of animal excitation is arranged, and proves that also Paris polyphylla Lysimachia sikokiana glycosides excitement uterus acts on dosage and is dependency relationships.
Present domestic relevant report of not seeing Paris polyphylla Lysimachia sikokiana glycosides extraction and separation method patent as yet.
Summary of the invention:
The purpose of this invention is to provide a kind of from the Paris polyphylla Lysimachia sikokiana method of extraction separation Paris polyphylla Lysimachia sikokiana glycosides, product Paris polyphylla Lysimachia sikokiana glycosides content height is measured content more than 98% through HPLC.
For achieving the above object, the present invention is by the following technical solutions:
A kind of from the Paris polyphylla Lysimachia sikokiana method of extraction separation Paris polyphylla Lysimachia sikokiana glycosides, it is characterized in that may further comprise the steps:
(1) gets the Paris polyphylla Lysimachia sikokiana and pulverize, add an amount of distilled water and biological enzyme normal temperature enzymolysis 2-3 days, get the enzymolysis raw material, add 5-10 and doubly measure 60-80% ethanolic soln supersound extraction 2-3 time, filter united extraction liquid;
(2) said extracted liquid adds activated carbon decolorizing, filters, and filtrate concentrating reclaimed ethanol, obtains concentrated solution;
(3) above-mentioned concentrated solution is used distilled water and aqueous ethanolic solution wash-out successively by polyamide column chromatography, collects alcohol eluen, and concentrate drying obtains crude product;
(4) adopt high-speed countercurrent chromatography to separate above-mentioned crude product and obtain highly purified Paris polyphylla Lysimachia sikokiana glycosides.
Biological enzyme is a cellulase in the described step (1), and consumption is the 0.5-1% of raw material weight, and the supersound extraction frequency is 35-50kHz.
Activated carbon dosage is 2-5% in the described step (2).
Ethanolic soln concentration is 50-70% in the described step (3).
The two-phase solvent system of described step (4) high speed adverse current chromatogram is methyl tertiary butyl ether-propyl carbinol-methanol-water, and volume ratio is 1: 2-4: 1: 3-5, on be stationary phase mutually, is moving phase mutually down, rotating speed is 750-950r/min.
Beneficial effect of the present invention:
(1) the inventive method is simple to operate, biological enzyme enzymeization, extraction yield height;
(2) the present invention adopts polyamide column chromatography and high-speed countercurrent chromatography separation and purification, has good separating effect, efficient, fast, characteristics such as product purity height.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1:
Get Paris polyphylla Lysimachia sikokiana 1kg, pulverize, add an amount of distilled water and 0.5% cellulase normal temperature enzymolysis 3 days, get the enzymolysis raw material, add 10 times of amount 70% ethanolic soln supersound extraction 2 times, ultrasonic frequency is 45kHz, filter, united extraction liquid adds 5% activated carbon decolorizing, filter, filtrate concentrating reclaimed ethanol, obtains concentrated solution, concentrated solution by polyamide column chromatography, with distilled water flush away impurity, is used 60% aqueous ethanolic solution wash-out earlier again, collect elutriant, concentrate drying obtains crude product; With methyl tertiary butyl ether-propyl carbinol-methanol-water is the two-phase solvent system, be 1: 3: 1 by volume: 3 preparations, solvent systems is placed the separating funnel jolting, leave standstill, tell upper and lower phase, on be stationary phase mutually, be moving phase mutually down, use phased soln crude product down, stationary phase is pumped in the chromatographic column, make in the post and be full of, restart main frame and rotate, the control rotating speed is 850r/min, goes into moving phase with the 1ml/min flow pump simultaneously, after treating that two-phase reaches running balance, sample introduction, ultraviolet detection is collected effluent liquid, rotary evaporation concentrates, the dry product 4.1g of getting, content 98.6%.
Embodiment 2:
Get Paris polyphylla Lysimachia sikokiana 2kg, pulverize, add an amount of distilled water and 1% cellulase normal temperature enzymolysis 2 days, get the enzymolysis raw material, add 5 times of amount 80% ethanolic soln supersound extraction 3 times, ultrasonic frequency is 35kHz, filter, united extraction liquid adds 2% activated carbon decolorizing, filter, filtrate concentrating reclaimed ethanol, obtains concentrated solution, concentrated solution by polyamide column chromatography, with distilled water flush away impurity, is used 50% aqueous ethanolic solution wash-out earlier again, collect elutriant, concentrate drying obtains crude product; With methyl tertiary butyl ether-propyl carbinol-methanol-water is the two-phase solvent system, be 1: 4: 1 by volume: 5 preparations, solvent systems is placed the separating funnel jolting, leave standstill, tell upper and lower phase, on be stationary phase mutually, be moving phase mutually down, use phased soln crude product down, stationary phase is pumped in the chromatographic column, make in the post and be full of, restart main frame and rotate, the control rotating speed is 800r/min, goes into moving phase with the 3ml/min flow pump simultaneously, after treating that two-phase reaches running balance, sample introduction, ultraviolet detection is collected effluent liquid, rotary evaporation concentrates, dry product 11.4g, the content 98.2% of getting.
Embodiment 3:
Get Paris polyphylla Lysimachia sikokiana 2kg, pulverize, add an amount of distilled water and 1% cellulase normal temperature enzymolysis 2 days, get the enzymolysis raw material, add 10 times of amount 60% ethanolic soln supersound extraction 2 times, ultrasonic frequency is 40kHz, filter, united extraction liquid adds 5% activated carbon decolorizing, filter, filtrate concentrating reclaimed ethanol, obtains concentrated solution, concentrated solution by polyamide column chromatography, with distilled water flush away impurity, is used 70% aqueous ethanolic solution wash-out earlier again, collect elutriant, concentrate drying obtains crude product; With methyl tertiary butyl ether-propyl carbinol-methanol-water is the two-phase solvent system, be 1: 3: 1 by volume: 5 preparations, solvent systems is placed the separating funnel jolting, leave standstill, tell upper and lower phase, on be stationary phase mutually, be moving phase mutually down, use phased soln crude product down, stationary phase is pumped in the chromatographic column, make in the post and be full of, restart main frame and rotate, the control rotating speed is 950r/min, goes into moving phase with the 2.5ml/min flow pump simultaneously, after treating that two-phase reaches running balance, sample introduction, ultraviolet detection is collected effluent liquid, rotary evaporation concentrates, dry product 9.3g, the content 98.5% of getting.
Embodiment 4:
Get Paris polyphylla Lysimachia sikokiana 5kg, pulverize, add an amount of distilled water and 0.8% cellulase normal temperature enzymolysis 2 days, get the enzymolysis raw material, add 7 times of amount 70% ethanolic soln supersound extraction 2 times, ultrasonic frequency is 50kHz, filter, united extraction liquid adds 3% activated carbon decolorizing, filter, filtrate concentrating reclaimed ethanol, obtains concentrated solution, concentrated solution by polyamide column chromatography, with distilled water flush away impurity, is used 60% aqueous ethanolic solution wash-out earlier again, collect elutriant, concentrate drying obtains crude product; With methyl tertiary butyl ether-propyl carbinol-methanol-water is the two-phase solvent system, be 1: 4: 1 by volume: 5 preparations, solvent systems is placed the separating funnel jolting, leave standstill, tell upper and lower phase, on be stationary phase mutually, be moving phase mutually down, use phased soln crude product down, stationary phase is pumped in the chromatographic column, make in the post and be full of, restart main frame and rotate, the control rotating speed is 850r/min, goes into moving phase with the 5ml/min flow pump simultaneously, after treating that two-phase reaches running balance, sample introduction, ultraviolet detection is collected effluent liquid, rotary evaporation concentrates, dry product 24.6g, the content 98.1% of getting.
Embodiment 5:
Get Paris polyphylla Lysimachia sikokiana 10kg, pulverize, add an amount of distilled water and 0.6% cellulase normal temperature enzymolysis 3 days, get the enzymolysis raw material, add 8 times of amount 80% ethanolic soln supersound extraction 3 times, ultrasonic frequency is 35kHz, filter, united extraction liquid adds 3% activated carbon decolorizing, filter, filtrate concentrating reclaimed ethanol, obtains concentrated solution, concentrated solution by polyamide column chromatography, with distilled water flush away impurity, is used 70% aqueous ethanolic solution wash-out earlier again, collect elutriant, concentrate drying obtains crude product; With methyl tertiary butyl ether-propyl carbinol-methanol-water is the two-phase solvent system, be 1: 3: 1 by volume: 5 preparations, solvent systems is placed the separating funnel jolting, leave standstill, tell upper and lower phase, on be stationary phase mutually, be moving phase mutually down, use phased soln crude product down, stationary phase is pumped in the chromatographic column, make in the post and be full of, restart main frame and rotate, the control rotating speed is 750r/min, goes into moving phase with the 5ml/min flow pump simultaneously, after treating that two-phase reaches running balance, sample introduction, ultraviolet detection is collected effluent liquid, rotary evaporation concentrates, dry product 42.9g, the content 98.8% of getting.
Claims (5)
1. the method for an extraction separation Paris polyphylla Lysimachia sikokiana glycosides from the Paris polyphylla Lysimachia sikokiana is characterized in that may further comprise the steps:
(1) gets the Paris polyphylla Lysimachia sikokiana and pulverize, add an amount of distilled water and biological enzyme normal temperature enzymolysis 2-3 days, get the enzymolysis raw material, add 5-10 and doubly measure 60-80% ethanolic soln supersound extraction 2-3 time, filter united extraction liquid;
(2) said extracted liquid adds activated carbon decolorizing, filters, and filtrate concentrating reclaimed ethanol, obtains concentrated solution;
(3) above-mentioned concentrated solution is used distilled water and aqueous ethanolic solution wash-out successively by polyamide column chromatography, collects alcohol eluen, and concentrate drying obtains crude product;
(4) adopt high-speed countercurrent chromatography to separate above-mentioned crude product and obtain highly purified Paris polyphylla Lysimachia sikokiana glycosides.
2. according to claim 1 a kind of from the Paris polyphylla Lysimachia sikokiana method of extraction separation Paris polyphylla Lysimachia sikokiana glycosides, it is characterized in that biological enzyme is a cellulase in the described step (1), consumption is the 0.5-1% of raw material weight, the supersound extraction frequency is 35-50kHz.
3. according to claim 1 a kind of from the Paris polyphylla Lysimachia sikokiana method of extraction separation Paris polyphylla Lysimachia sikokiana glycosides, it is characterized in that activated carbon dosage is 2-5% in the described step (2).
4. according to claim 1 a kind of from the Paris polyphylla Lysimachia sikokiana method of extraction separation Paris polyphylla Lysimachia sikokiana glycosides, it is characterized in that ethanolic soln concentration is 50-70% in the described step (3).
5. according to claim 1 a kind of from the Paris polyphylla Lysimachia sikokiana method of extraction separation Paris polyphylla Lysimachia sikokiana glycosides, the two-phase solvent system that it is characterized in that described step (4) high speed adverse current chromatogram is methyl tertiary butyl ether-propyl carbinol-methanol-water, volume ratio is 1: 2-4: 1: 3-5, on be stationary phase mutually, be moving phase mutually down, rotating speed is 750-950r/min.
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| CN2011101178402A CN102234307A (en) | 2011-05-06 | 2011-05-06 | Method for extracting and separating pardifomoside from Lysimachia paridiformis |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827240A (en) * | 2012-09-20 | 2012-12-19 | 南京泽朗农业发展有限公司 | Method for extracting and separating thorn leaf pink glycosides A |
| CN105963479A (en) * | 2016-06-17 | 2016-09-28 | 广州中大南沙科技创新产业园有限公司 | Method for extracting paris polyphylla saponin |
| CN108531318A (en) * | 2018-07-21 | 2018-09-14 | 安溪县凤城建金产品外观设计服务中心 | A kind of preparation process of the soap containing paris polyphylla extract |
| CN110663709A (en) * | 2019-11-15 | 2020-01-10 | 中南民族大学 | Preparation method and application of paris polyphylla extractive solution |
| CN112618584A (en) * | 2020-12-15 | 2021-04-09 | 博奥生物集团有限公司 | Application of four-tile extract in preparing medicine for resisting hepatitis B virus and/or preventing and treating hepatitis B |
-
2011
- 2011-05-06 CN CN2011101178402A patent/CN102234307A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827240A (en) * | 2012-09-20 | 2012-12-19 | 南京泽朗农业发展有限公司 | Method for extracting and separating thorn leaf pink glycosides A |
| CN105963479A (en) * | 2016-06-17 | 2016-09-28 | 广州中大南沙科技创新产业园有限公司 | Method for extracting paris polyphylla saponin |
| CN108531318A (en) * | 2018-07-21 | 2018-09-14 | 安溪县凤城建金产品外观设计服务中心 | A kind of preparation process of the soap containing paris polyphylla extract |
| CN110663709A (en) * | 2019-11-15 | 2020-01-10 | 中南民族大学 | Preparation method and application of paris polyphylla extractive solution |
| CN112618584A (en) * | 2020-12-15 | 2021-04-09 | 博奥生物集团有限公司 | Application of four-tile extract in preparing medicine for resisting hepatitis B virus and/or preventing and treating hepatitis B |
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Application publication date: 20111109 |