CN102786563A - Preparation process for separating three kinds of stilbene glucoside monomeric compounds from rhubarb - Google Patents

Preparation process for separating three kinds of stilbene glucoside monomeric compounds from rhubarb Download PDF

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CN102786563A
CN102786563A CN2012103250993A CN201210325099A CN102786563A CN 102786563 A CN102786563 A CN 102786563A CN 2012103250993 A CN2012103250993 A CN 2012103250993A CN 201210325099 A CN201210325099 A CN 201210325099A CN 102786563 A CN102786563 A CN 102786563A
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rhubarb
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岳会兰
赵晓辉
韩发
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Northwest Institute of Plateau Biology of CAS
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Abstract

The invention relates to preparation process for separating three kinds of stilbene glucoside monomeric compounds from rhubarb. The process comprises the steps of (1) conducting heat reflux extraction on crushed rhubarb roots at a temperature between 40 DEG C and 80 DEG C by using alcohol, and merging to obtain an extracting solution; (2) conducting reduced pressure distillation drying on the extracting solution to obtain rhubarb extracts; (3) dissolving rhubarb extracts with deionized water, and conducting extraction with petroleum ether and ethyl acetate sequentially so as to obtain rhubarb aqueous extracts which are residue aqueous phase parts; (4) eluting nonpolar macroporous resin columns on aqueous rhubarb extracts with ethanol water to obtain an eluent containing stilbene glucoside substances, and drying the eluent by distillation to obtain crude stilbene glucoside extracts; and (5) separating crude stilbene glucoside extracts in a chloroform-normal butanol-methanol-water system by using a high-speed counter-current chromatography device, so that trans-rhapontin, cis-rhapontin and trans-deoxidized rhapontin can be obtained respectively. The process is simple, fast and low in cost.

Description

The preparation method who from rheum officinale, separates three kinds of toluylene glycoside monomeric compounds
Technical field
The present invention relates to the preparation method of trans-rhapontin, cis-rhapontin and three kinds of toluylene glycosides of trans-desoxyrhaponticin monomeric compound, relate in particular to the preparation method who from rheum officinale, separates three kinds of toluylene glycoside monomeric compounds.
Background technology
Stilbene glucoside is claimed the stilbene polyphenol again, belongs to poly-hydroxy stilbene compound (polyhydrostilbenes), extensively is present in mosses and the senior plant.Stilbene glucoside is accredited as a kind of phytoalexin, is produced under unfavourable condition such as fungi infestation, uviolizing, physical abuse by plant.Discover that stilbene glucoside has multiple physiologically active and pharmaceutical use, reducing blood-fat, anti-ageing, suppress aspect such as tumour and demonstrate functionally, this is showing its important research and development especially and is being worth in the society of current aging day by day.
High speed adverse current chromatogram (High-speed Countercurrent Chromatography is called for short HSCCC) is a liquid liquid distribution chromatography technology of not using solid-state supporter or carrier, has applied range, and flexibility is good; Easy and simple to handle, easy master; The recovery is high; Favorable reproducibility; Separation efficiency is high, the advantage that fractional dose is bigger, and it has overcome solid phase carrier to shortcomings such as the adsorption losses of sample, sex change, and sample recovery rate is high, be widely used in the Analysis and Identification of natural medicinal ingredients and separated preparation.Compare with other column chromatography, it has overcome shortcomings such as the sample absorption that the stationary phase carrier brings, loss, pollution and peak shape hangover.Domestic and international research shows; The HSCCC technology from agricultural-food, medium-height grass medicines natural products separation and purification with prepared hundreds of monomer components, these compositions comprise materials such as flavonoid, alkaloids, anthraquinone class, saponins, Macrolide, Polyphenols, catechin, polyose, glycoprotein analog.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method who from rheum officinale, separates three kinds of toluylene glycoside monomeric compounds easy, quick, with low cost.
For addressing the above problem, the preparation method who from rheum officinale, separates three kinds of toluylene glycoside monomeric compounds of the present invention may further comprise the steps:
⑴ it is that 30% ~ 95% alcohol carries out thermal backflow and extracts under 40 ~ 80 ℃ that the big xanthorrhiza that will pulverize adopts mass concentration, extracts 1 ~ 4 time, each 1 ~ 3h, and merging obtains extracting solution;
⑵ be that 30 ~ 80 ℃, pressure are evaporated under reduced pressure under the condition of 0.05 ~ 0.08MPa with said extracting solution in temperature, obtains Radix Et Rhizoma Rhei extract;
⑶ use deionized water dissolving earlier with said Radix Et Rhizoma Rhei extract, uses sherwood oil, ethyl acetate extraction 2 ~ 10 times more successively, and the residue aqueous portion is the rheum officinale aqueous extract;
⑷ with non-polar macroporous resin post on the said rheum officinale aqueous extract; With 2 ~ 50 times of column volumes, mass concentration is 50 ~ 95% aqueous ethanolic solution wash-outs; Obtain containing the elutriant of toluylene glycoside material; This elutriant is that 30 ~ 80 ℃, pressure are evaporate to dryness under the condition of 0.05 ~ 0.08MPa in temperature, promptly gets the stilbene glucoside crude extract;
⑸ said stilbene glucoside crude extract adopts high speed adverse current chromatogram equipment; In chloroform-propyl carbinol-methanol-water system, be that 500 ~ 1000r/min, temperature are that 20 ~ 50 ℃ condition is separated it, can obtain trans ponticin (trans-rhapontin), cis ponticin (cis-rhapontin), three kinds of toluylene glycosides of trans Rhapontin, deoxy-(trans-desoxyrhaponticin) material respectively with rotating speed.
Figure 2012103250993100002DEST_PATH_IMAGE001
The mass volume ratio of Radix Et Rhizoma Rhei extract and said deionized water is 1:1 ~ 10 among the said step ⑶.
The volume ratio of chloroform, propyl carbinol, methyl alcohol, water is 4:0.1 ~ 2:3:1 ~ 5 in said step ⑸ chloroform-propyl carbinol-methanol-water system.
The present invention compared with prior art has the following advantages:
1, the present invention adopts high speed adverse current chromatogram (HSCCC) stripping technique, compares with the conventional post chromatographic separation technology, has not only shortened disengaging time effectively, has reduced organic solvent consumption and the energy consumption in the technological process.
2, flash liberation of the present invention three kinds of high purity toluylene glycoside monomeric compounds, the stable in properties that can obtain simultaneously, purity high (can reach more than 97%) can be applicable to medicine, reference material, protective foods and health medicine etc.
3, the present invention adopts the HSCCC stripping technique, this method circulation ratio is high, simple, fast, can reduce the sample loss problem in traditional solid-liquid separation effectively.
4, because the present invention adopts the abundant big xanthorrhiza of raw material resources amount as raw material, therefore, reduced production cost effectively.
Embodiment
Embodiment 1From rheum officinale, separate the preparation method of three kinds of toluylene glycoside monomeric compounds, may further comprise the steps:
⑴ it is that 30% alcohol carries out thermal backflow and extracts under 40 ℃ that the big xanthorrhiza that will pulverize adopts mass concentration, extracts 1 time, each 1h, and merging obtains extracting solution.
⑵ be that 30 ℃, pressure are evaporated under reduced pressure under the condition of 0.05MPa with extracting solution in temperature, obtains Radix Et Rhizoma Rhei extract.
⑶ use deionized water dissolving earlier with Radix Et Rhizoma Rhei extract, uses sherwood oil, ethyl acetate extraction 2 times more successively, and the residue aqueous portion is the rheum officinale aqueous extract; Wherein the mass volume ratio of Radix Et Rhizoma Rhei extract and deionized water (kg/ml) is 1:1.
⑷ with non-polar macroporous resin post on the rheum officinale aqueous extract; Using 2 times of column volumes, mass concentrations is 50% aqueous ethanolic solution wash-out; Obtain containing the elutriant of toluylene glycoside material; This elutriant is that 30 ℃, pressure are evaporated under reduced pressure under the condition of 0.05MPa in temperature, promptly gets the stilbene glucoside crude extract.
⑸ stilbene glucoside crude extract adopts high speed adverse current chromatogram equipment; In chloroform-propyl carbinol-methanol-water system be that 500r/min, temperature are that 20 ℃ condition is separated it, can obtain trans-rhapontin, cis-rhapontin, three kinds of toluylene glycosides of trans-desoxyrhaponticin material respectively with the rotating speed.
Wherein: the volume ratio (ml/ml) of chloroform, propyl carbinol, methyl alcohol, water is 4:0.1:3:1 in chloroform-propyl carbinol-methanol-water system.
Embodiment 2From rheum officinale, separate the preparation method of three kinds of toluylene glycoside monomeric compounds, may further comprise the steps:
⑴ it is that 95% alcohol carries out thermal backflow and extracts under 80 ℃ that the big xanthorrhiza that will pulverize adopts mass concentration, extracts 4 times, each 3h, and merging obtains extracting solution.
⑵ be that 80 ℃, pressure are evaporated under reduced pressure under the condition of 0.08MPa with extracting solution in temperature, obtains Radix Et Rhizoma Rhei extract.
⑶ use deionized water dissolving earlier with Radix Et Rhizoma Rhei extract, uses sherwood oil, ethyl acetate extraction 10 times more successively, and the residue aqueous portion is the rheum officinale aqueous extract; Wherein the mass volume ratio of Radix Et Rhizoma Rhei extract and deionized water (kg/ml) is 1:10.
⑷ with non-polar macroporous resin post on the rheum officinale aqueous extract; Using 50 times of column volumes, mass concentrations is 95% aqueous ethanolic solution wash-out; Obtain containing the elutriant of toluylene glycoside material; This elutriant is that 80 ℃, pressure are evaporated under reduced pressure under the condition of 0.08MPa in temperature, promptly gets the stilbene glucoside crude extract.
⑸ stilbene glucoside crude extract adopts high speed adverse current chromatogram equipment; In chloroform-propyl carbinol-methanol-water system be that 1000r/min, temperature are that 50 ℃ condition is separated it, can obtain trans-rhapontin, cis-rhapontin, three kinds of toluylene glycosides of trans-desoxyrhaponticin material respectively with the rotating speed.
Wherein: the volume ratio (ml/ml) of chloroform, propyl carbinol, methyl alcohol, water is 4:2:3:5 in chloroform-propyl carbinol-methanol-water system.
Embodiment 3From rheum officinale, separate the preparation method of three kinds of toluylene glycoside monomeric compounds, may further comprise the steps:
⑴ it is that 80% alcohol carries out thermal backflow and extracts under 70 ℃ that the big xanthorrhiza that will pulverize adopts mass concentration, extracts 3 times, each 2h, and merging obtains extracting solution.
⑵ be that 70 ℃, pressure are evaporated under reduced pressure under the condition of 0.06MPa with extracting solution in temperature, obtains Radix Et Rhizoma Rhei extract.
⑶ use deionized water dissolving earlier with Radix Et Rhizoma Rhei extract, uses sherwood oil, ethyl acetate extraction 10 times more successively, and the residue aqueous portion is the rheum officinale aqueous extract; Wherein the mass volume ratio of Radix Et Rhizoma Rhei extract and deionized water (kg/ml) is 1:8.
⑷ with non-polar macroporous resin post on the rheum officinale aqueous extract; Using 50 times of column volumes, mass concentrations is 90% aqueous ethanolic solution wash-out; Obtain containing the elutriant of toluylene glycoside material; This elutriant is that 70 ℃, pressure are evaporated under reduced pressure under the condition of 0.06MPa in temperature, promptly gets the stilbene glucoside crude extract.
⑸ stilbene glucoside crude extract adopts high speed adverse current chromatogram equipment; In chloroform-propyl carbinol-methanol-water system be that 950r/min, temperature are that 40 ℃ condition is separated it, can obtain trans-rhapontin, cis-rhapontin, three kinds of toluylene glycosides of trans-desoxyrhaponticin material respectively with the rotating speed.
Wherein: the volume ratio (ml/ml) of chloroform, propyl carbinol, methyl alcohol, water is 4:0.2:3:4 in chloroform-propyl carbinol-methanol-water system.
Embodiment 4From rheum officinale, separate the preparation method of three kinds of toluylene glycoside monomeric compounds, may further comprise the steps:
⑴ it is that 60% alcohol carries out thermal backflow and extracts under 50 ℃ that the big xanthorrhiza that will pulverize adopts mass concentration, extracts 2 times, each 2h, and merging obtains extracting solution.
⑵ be that 60 ℃, pressure are evaporated under reduced pressure under the condition of 0.07MPa with extracting solution in temperature, obtains Radix Et Rhizoma Rhei extract.
⑶ use deionized water dissolving earlier with Radix Et Rhizoma Rhei extract, uses sherwood oil, ethyl acetate extraction 8 times more successively, and the residue aqueous portion is the rheum officinale aqueous extract; Wherein the mass volume ratio of Radix Et Rhizoma Rhei extract and deionized water (kg/ml) is 1:5.
⑷ with non-polar macroporous resin post on the rheum officinale aqueous extract; Using 20 times of column volumes, mass concentrations is 85% aqueous ethanolic solution wash-out; Obtain containing the elutriant of toluylene glycoside material; This elutriant is that 60 ℃, pressure are evaporated under reduced pressure under the condition of 0.07MPa in temperature, promptly gets the stilbene glucoside crude extract.
⑸ stilbene glucoside crude extract adopts high speed adverse current chromatogram equipment; In chloroform-propyl carbinol-methanol-water system be that 950r/min, temperature are that 35 ℃ condition is separated it, can obtain trans-rhapontin, cis-rhapontin, three kinds of toluylene glycosides of trans-desoxyrhaponticin material respectively with the rotating speed.
Wherein: the volume ratio (ml/ml) of chloroform, propyl carbinol, methyl alcohol, water is 4:1:3:2 in chloroform-propyl carbinol-methanol-water system.
Embodiment 5From rheum officinale, separate the preparation method of three kinds of toluylene glycoside monomeric compounds, may further comprise the steps:
⑴ it is that 50% alcohol carries out thermal backflow and extracts under 50 ℃ that the big xanthorrhiza that will pulverize adopts mass concentration, extracts 3 times, each 3h, and merging obtains extracting solution.
⑵ be that 70 ℃, pressure are evaporated under reduced pressure under the condition of 0.05MPa with extracting solution in temperature, obtains Radix Et Rhizoma Rhei extract.
⑶ use deionized water dissolving earlier with Radix Et Rhizoma Rhei extract, uses sherwood oil, ethyl acetate extraction 6 times more successively, and the residue aqueous portion is the rheum officinale aqueous extract; Wherein the mass volume ratio of Radix Et Rhizoma Rhei extract and deionized water (kg/ml) is 1:4.
⑷ with non-polar macroporous resin post on the rheum officinale aqueous extract; Using 30 times of column volumes, mass concentrations is 70% aqueous ethanolic solution wash-out; Obtain containing the elutriant of toluylene glycoside material, this elutriant is an evaporated under reduced pressure under 70 ℃, the condition of 0.05MPa in temperature, promptly gets the stilbene glucoside crude extract.
⑸ stilbene glucoside crude extract adopts high speed adverse current chromatogram equipment; In chloroform-propyl carbinol-methanol-water system be that 800r/min, temperature are that 30 ℃ condition is separated it, can obtain trans-rhapontin, cis-rhapontin, three kinds of toluylene glycosides of trans-desoxyrhaponticin material respectively with the rotating speed.
Wherein: the volume ratio (ml/ml) of chloroform, propyl carbinol, methyl alcohol, water is 4:0.5:3:2 in chloroform-propyl carbinol-methanol-water system.
Embodiment 6From rheum officinale, separate the preparation method of three kinds of toluylene glycoside monomeric compounds, may further comprise the steps:
⑴ it is that 75% alcohol carries out thermal backflow and extracts under 60 ℃ that the big xanthorrhiza that will pulverize adopts mass concentration, extracts 3 times, each 2h, and merging obtains extracting solution.
⑵ be that 65 ℃, pressure are evaporated under reduced pressure under the condition of 0.07MPa with extracting solution in temperature, obtains Radix Et Rhizoma Rhei extract.
⑶ use deionized water dissolving earlier with Radix Et Rhizoma Rhei extract, uses sherwood oil, ethyl acetate extraction 6 times more successively, and the residue aqueous portion is the rheum officinale aqueous extract; Wherein the mass volume ratio of Radix Et Rhizoma Rhei extract and deionized water (kg/ml) is 1:2.
⑷ with non-polar macroporous resin post on the rheum officinale aqueous extract; Using 25 times of column volumes, mass concentrations is 90% aqueous ethanolic solution wash-out; Obtain containing the elutriant of toluylene glycoside material; This elutriant is that 65 ℃, pressure are evaporated under reduced pressure under the condition of 0.07MPa in temperature, promptly gets the stilbene glucoside crude extract.
⑸ stilbene glucoside crude extract adopts high speed adverse current chromatogram equipment; In chloroform-propyl carbinol-methanol-water system be that 700r/min, temperature are that 45 ℃ condition is separated it, can obtain trans-rhapontin, cis-rhapontin, three kinds of toluylene glycosides of trans-desoxyrhaponticin material respectively with the rotating speed.
Wherein: the volume ratio (ml/ml) of chloroform, propyl carbinol, methyl alcohol, water is 4:0.1:3:5 in chloroform-propyl carbinol-methanol-water system.
Embodiment 7From rheum officinale, separate the preparation method of three kinds of toluylene glycoside monomeric compounds, may further comprise the steps:
⑴ it is that 90% alcohol carries out thermal backflow and extracts under 50 ℃ that the big xanthorrhiza that will pulverize adopts mass concentration, extracts 3 times, each 3h, and merging obtains extracting solution.
⑵ be that 55 ℃, pressure are evaporated under reduced pressure under the condition of 0.08MPa with extracting solution in temperature, obtains Radix Et Rhizoma Rhei extract.
⑶ use deionized water dissolving earlier with Radix Et Rhizoma Rhei extract, uses sherwood oil, ethyl acetate extraction 4 times more successively, and the residue aqueous portion is the rheum officinale aqueous extract; Wherein the mass volume ratio of Radix Et Rhizoma Rhei extract and deionized water (kg/ml) is 1:3.
⑷ with non-polar macroporous resin post on the rheum officinale aqueous extract; Using 10 times of column volumes, mass concentrations is 55% aqueous ethanolic solution wash-out; Obtain containing the elutriant of toluylene glycoside material; This elutriant is that 55 ℃, pressure are evaporated under reduced pressure under the condition of 0.08MPa in temperature, promptly gets the stilbene glucoside crude extract.
⑸ stilbene glucoside crude extract adopts high speed adverse current chromatogram equipment; In chloroform-propyl carbinol-methanol-water system be that 750r/min, temperature are that 25 ℃ condition is separated it, can obtain trans-rhapontin, cis-rhapontin, three kinds of toluylene glycosides of trans-desoxyrhaponticin material respectively with the rotating speed.
Wherein: the volume ratio (ml/ml) of chloroform, propyl carbinol, methyl alcohol, water is 4:0.5:3:1 in chloroform-propyl carbinol-methanol-water system.
Embodiment 8From rheum officinale, separate the preparation method of three kinds of toluylene glycoside monomeric compounds, may further comprise the steps:
⑴ it is that 80% alcohol carries out thermal backflow and extracts under 65 ℃ that the big xanthorrhiza that will pulverize adopts mass concentration, extracts 3 times, each 1.5h, and merging obtains extracting solution.
⑵ be that 65 ℃, pressure are evaporated under reduced pressure under the condition of 0.06MPa with extracting solution in temperature, obtains Radix Et Rhizoma Rhei extract.
⑶ use deionized water dissolving earlier with Radix Et Rhizoma Rhei extract, uses sherwood oil, ethyl acetate extraction 10 times more successively, and the residue aqueous portion is the rheum officinale aqueous extract; Wherein the mass volume ratio of Radix Et Rhizoma Rhei extract and deionized water (kg/ml) is 1:6.
⑷ with non-polar macroporous resin post on the rheum officinale aqueous extract; Using 25 times of column volumes, mass concentrations is 90% aqueous ethanolic solution wash-out; Obtain containing the elutriant of toluylene glycoside material; This elutriant is that 65 ℃, pressure are evaporated under reduced pressure under the condition of 0.07MPa in temperature, promptly gets the stilbene glucoside crude extract.
⑸ stilbene glucoside crude extract adopts high speed adverse current chromatogram equipment; In chloroform-propyl carbinol-methanol-water system be that 900r/min, temperature are that 35 ℃ condition is separated it, can obtain trans-rhapontin, cis-rhapontin, three kinds of toluylene glycosides of trans-desoxyrhaponticin material respectively with the rotating speed.
Wherein: the volume ratio (ml/ml) of chloroform, propyl carbinol, methyl alcohol, water is 4:1.2:3:4 in chloroform-propyl carbinol-methanol-water system.
Embodiment 9From rheum officinale, separate the preparation method of three kinds of toluylene glycoside monomeric compounds, may further comprise the steps:
⑴ it is that 70% alcohol carries out thermal backflow and extracts under 75 ℃ that the big xanthorrhiza that will pulverize adopts mass concentration, extracts 2 times, each 2h, and merging obtains extracting solution.
⑵ be that 65 ℃, pressure are evaporated under reduced pressure under the condition of 0.06MPa with extracting solution in temperature, obtains Radix Et Rhizoma Rhei extract.
⑶ use deionized water dissolving earlier with Radix Et Rhizoma Rhei extract, uses sherwood oil, ethyl acetate extraction 10 times more successively, and the residue aqueous portion is the rheum officinale aqueous extract; Wherein the mass volume ratio of Radix Et Rhizoma Rhei extract and deionized water (kg/ml) is 1:6.
⑷ with non-polar macroporous resin post on the rheum officinale aqueous extract; Using 25 times of column volumes, mass concentrations is 90% aqueous ethanolic solution wash-out; Obtain containing the elutriant of toluylene glycoside material; This elutriant is that 65 ℃, pressure are evaporated under reduced pressure under the condition of 0.07MPa in temperature, promptly gets the stilbene glucoside crude extract.
⑸ stilbene glucoside crude extract adopts high speed adverse current chromatogram equipment; In chloroform-propyl carbinol-methanol-water system be that 900r/min, temperature are that 35 ℃ condition is separated it, can obtain trans-rhapontin, cis-rhapontin, three kinds of toluylene glycosides of trans-desoxyrhaponticin material respectively with the rotating speed.
Wherein: the volume ratio (ml/ml) of chloroform, propyl carbinol, methyl alcohol, water is 4:0.2:3:2 in chloroform-propyl carbinol-methanol-water system.

Claims (3)

1. from rheum officinale, separate the preparation method of three kinds of toluylene glycoside monomeric compounds, may further comprise the steps:
⑴ it is that 30% ~ 95% alcohol carries out thermal backflow and extracts under 40 ~ 80 ℃ that the big xanthorrhiza that will pulverize adopts mass concentration, extracts 1 ~ 4 time, each 1 ~ 3h, and merging obtains extracting solution;
⑵ be that 30 ~ 80 ℃, pressure are evaporated under reduced pressure under the condition of 0.05 ~ 0.08MPa with said extracting solution in temperature, obtains Radix Et Rhizoma Rhei extract;
⑶ use deionized water dissolving earlier with said Radix Et Rhizoma Rhei extract, uses sherwood oil, ethyl acetate extraction 2 ~ 10 times more successively, and the residue aqueous portion is the rheum officinale aqueous extract;
⑷ with non-polar macroporous resin post on the said rheum officinale aqueous extract; With 2 ~ 50 times of column volumes, mass concentration is 50 ~ 95% aqueous ethanolic solution wash-outs; Obtain containing the elutriant of toluylene glycoside material; This elutriant is that 30 ~ 80 ℃, pressure are evaporate to dryness under the condition of 0.05 ~ 0.08MPa in temperature, promptly gets the stilbene glucoside crude extract;
⑸ said stilbene glucoside crude extract adopts high speed adverse current chromatogram equipment; In chloroform-propyl carbinol-methanol-water system, be that 500 ~ 1000r/min, temperature are that 20 ~ 50 ℃ condition is separated it, can obtain trans ponticin, cis ponticin, three kinds of toluylene glycosides of trans Rhapontin, deoxy-material respectively with rotating speed.
2. the preparation method who from rheum officinale, separates three kinds of toluylene glycoside monomeric compounds as claimed in claim 1, it is characterized in that: the mass volume ratio of Radix Et Rhizoma Rhei extract and said deionized water is 1:1 ~ 10 among the said step ⑶.
3. the preparation method who from rheum officinale, separates three kinds of toluylene glycoside monomeric compounds as claimed in claim 1, it is characterized in that: the volume ratio of chloroform, propyl carbinol, methyl alcohol, water is 4:0.1 ~ 2:3:1 ~ 5 in said step ⑸ chloroform-propyl carbinol-methanol-water system.
CN2012103250993A 2012-09-05 2012-09-05 Preparation process for separating three kinds of stilbene glucoside monomeric compounds from rhubarb Pending CN102786563A (en)

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CN103351411A (en) * 2013-07-19 2013-10-16 中国科学院西北高原生物研究所 Method for preparing five phenylpropanoid glycoside monomeric compounds in Lamiophlomis rotata (Benth) Kudo through separation
CN103408613A (en) * 2013-07-22 2013-11-27 中国科学院西北高原生物研究所 Preparation method for chemical reference substances of anthraquinone glucoside and stibene glucoside in rheum officinale medicinal material
CN103800483A (en) * 2014-02-26 2014-05-21 天津中新药业集团股份有限公司达仁堂制药厂 Method for preparing traditional Chinese medicinal extract capable of diminishing edema, removing toxicity, purging and stopping bleeding
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CN106674303A (en) * 2016-11-18 2017-05-17 中国科学院西北高原生物研究所 Method for extracting tetrahydroxystilbene-glucoside compound Desoxyrhaponticin reference substance from rheum palmatum l
CN107474083A (en) * 2017-07-13 2017-12-15 中国科学院西北高原生物研究所 The novel preparation method of diphenylethylene and phenyl propyl ketone class chemical reference substance in a kind of rhubarb medicinal material
CN112521434A (en) * 2020-12-07 2021-03-19 山东大学 High-efficiency preparation method of stilbene glucoside in polygonum multiflorum

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