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Diphenyl ethylene glycosides derivatives

A technology of stilbene glycosides and ethanol, which is applied in the field of medicine, can solve the problems that the purity of stilbene glycosides is far from meeting the quality requirements, cannot meet industrial production, and the process is cumbersome, etc., and achieves the improvement of large dosage, less impurities, and drug efficacy. exact effect

Inactive Publication Date: 2008-09-03
NANJING CHIA TAI TIANQING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These documents are also based on basic research carried out in laboratory research, and the amount of resin used is generally only a few grams, which is still incomparable with industrial production processes, and the purity of the stilbene glycosides obtained is far from that of monomers. Quality requirements
[0008] In addition, Chinese patent ZL 98120290.X discloses a method for preparing stilbene glycosides, which involves destructively cutting the chromatographic column used for separation and purification, and then performing sampling and separation. The process is cumbersome and the cost is extremely high, which is also typical. The method of preparing micro samples in the laboratory cannot meet the requirements of industrial production

Method used

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  • Diphenyl ethylene glycosides derivatives
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Examples

Experimental program
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Effect test

Embodiment 1

[0049] Take 100kg of dried Polygonum multiflorum, cut into thin slices of 1-3mm, put it into a heat reflux extraction tank, add 10 times the amount of water and an appropriate amount of sodium sulfite, adjust the pH of the extract to 7.6, heat and reflux extraction 3 times, 1 hour each time, Combine the extracts, filter, and collect the filtrate. Pass the filtrate through a HPD-400 macroporous adsorption resin column, add 500L of water to elute, then add 80% ethanol to elute, collect the eluate containing stilbene glycosides, a total of 200L, concentrate under reduced pressure at 60°C to 10L, add ethyl acetate The ester was extracted 3 times, each time using 10 L, and the ethyl acetate solution was concentrated under reduced pressure at 60°C to dryness to obtain 2.5 kg of the crude stilbene glycoside extract.

[0050] Take the above crude extract, add 5.0L of ethanol, heat and stir to make it fully dissolved, filter, and pass the filtrate through a 200-300 mesh neutral alumina...

Embodiment 2

[0053] Take 100kg of dried Radix Polygoni Multiflori, crush it into a coarse powder, put it into a heat reflux extraction tank, add 8 times the amount of water and an appropriate amount of sodium bisulfite, adjust the pH of the extract to 7.5, heat and reflux extraction twice, each time for 2 hours, Combine the extracts, filter, and collect the filtrate. Pass the filtrate through HPD-100 macroporous adsorption resin column, add 600L of water to elute, add 70% ethanol to elute, collect the eluate containing stilbene glycosides, total 300L, concentrate under reduced pressure at 70°C to 15L, add n-butyl Alcohol extraction was carried out twice, with 15 L each time, concentrated under reduced pressure at 80°C, and concentrated n-butanol to dryness to obtain 2.3 kg of crude stilbene glycoside extract.

[0054] Take the above crude extract, add 8.0 L of ethyl acetate, heat and stir to make it fully dissolved, filter, pass the filtrate through a 200-300 mesh silica gel chromatography...

Embodiment 3

[0057] Take 120kg of dried Polygonum multiflorum, crush it into coarse powder, put it into a hot reflux extraction tank, add 7 times the amount of water and an appropriate amount of sodium carbonate, adjust the pH of the extract to 7.8, heat and reflux for 3 times, each time for 1.5 hours, and combine the extractions liquid, filtered, and the filtrate collected. Pass the filtrate through the AB-8 macroporous adsorption resin column, add 600L of water to elute, then add 90% ethanol to elute, collect the eluate containing stilbene glycosides, a total of 320L, concentrate under reduced pressure at 70°C to 20L, add ethyl acetate The ester was extracted 3 times with 20 L each time, concentrated under reduced pressure at 80°C, and the ethyl acetate was concentrated to dryness to obtain 2.92 kg of crude stilbene glycoside extract.

[0058] Take the above crude extract, add 12L of acetone, heat and stir to fully dissolve, filter, and pass the filtrate through a 200-300 mesh neutral al...

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PUM

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Abstract

The invention relates to a new type 2, 3, 5, 4'- tetra-hydroxyl diphenyl ethylene-2-O-beta-D-glucoside crystal, a method for making same, and pharmaceutical compositions containing the crystal. The content of the crystal is 90-99. 9tested by high performance liquid chromatography, and the stilbene glucoside crystal of high-purity is obtained by abstracting fleece-flower root, extracting with an organic solvent, separating by column chromatography and crystallizing in appropriate dissolvent. The preparing process provides high yield, low cost, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a separation and purification process of effective monomer 2,3,5,4'-tetrahydroxystilbene-2-O-β-D-glucoside in Radix Polygoni Multiflori; also relates to 2,3,5 , Crystal of 4'-tetrahydroxystilbene-2-O-β-D-glucoside, preparation method thereof, and pharmaceutical composition containing it as main component. Background technique [0002] Polygonum multiflorum is the tuber root of Polygonum multiflorum Thunb., which is a commonly used traditional Chinese medicine with a long history of medicinal use. A large number of research results at home and abroad show that Polygonum multiflorum has many functions such as immune regulation, liver protection, anti-oxidation, anti-tumor, and blood fat reduction. pharmacological activity. With the deepening of research, the research on its chemical composition has become more and more clear. A large number of studies have shown that the main role ...

Claims

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Application Information

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IPC IPC(8): C07H15/203A61K31/7034A61K36/704A61P39/06A61K125/00
Inventor 杨永安王鸯
Owner NANJING CHIA TAI TIANQING PHARMA
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