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Preparation method of Ombuoside H

A pedicle, supercritical technology, applied to the preparation of sugar derivatives, chemical instruments and methods, steroids, etc., to achieve the effects of less pollution, large-scale production operations, and low energy consumption

Inactive Publication Date: 2012-10-03
SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the prior art, there is no report on the preparation process applicable to the industrialized large-scale production of high-purity peduroside H

Method used

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  • Preparation method of Ombuoside H

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Get 10Kg of Phytophthora rhizome coarse powder, add to CO 2 In the supercritical extractor, n-butanol is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 2%, the extraction pressure is 20MPa, the temperature is 40°C, and CO 2 The flow rate is 1ml / g crude drug·min, the extraction time is 80min, and the extract is obtained, which is added to a D101 macroporous adsorption resin column for adsorption, eluted with 60% ethanol, and 3 times the column volume eluate is collected, and the solvent is recovered under reduced pressure and dried , added to a silica gel chromatography column, and eluted with methanol-chloroform mixed solvent, the ratio of methanol to chloroform in the mixed solvent is 1:1, the eluent is collected in fractions by column volume, and the 3-7 column volume The eluate was concentrated, added acetone to crystallize, separated, washed, and dried to obtain 20.8g of white powder peduroside H, which was detect...

Embodiment 2

[0027] Get 10Kg of Phytophthora rhizome coarse powder, add to CO 2 In the supercritical extractor, n-butanol is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 4%, the extraction pressure is 40MPa, the temperature is 60°C, and the CO 2 The flow rate is 3ml / g crude drug·min, the extraction time is 150min, and the extract is obtained, which is added to a D102 macroporous adsorption resin column for adsorption, eluted with 80% ethanol, and 8 times the column volume eluate is collected, and the solvent is recovered under reduced pressure and dried , added to a silica gel chromatography column, and eluted with methanol-chloroform mixed solvent, the ratio of methanol to chloroform in the mixed solvent is 1:1, the eluent is collected in fractions by column volume, and the 3-7 column volume The eluate was concentrated, added acetone to crystallize, separated, washed, and dried to obtain 23.4g of white powder phytoglucoside H, which w...

Embodiment 3

[0029] Get 10Kg of Phytophthora rhizome coarse powder, add to CO 2 In the supercritical extractor, n-butanol is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 3%, the extraction pressure is 30MPa, the temperature is 50°C, and CO 2 The flow rate is 2ml / g crude drug·min, the extraction time is 100min, and the extract is obtained, which is added to an AB8 macroporous adsorption resin column for adsorption, eluted with 70% ethanol, and 5 times the column volume eluate is collected, and the solvent is recovered under reduced pressure and dried , added to a silica gel chromatography column, and eluted with methanol-chloroform mixed solvent, the ratio of methanol to chloroform in the mixed solvent is 1:1, the eluent is collected in fractions by column volume, and the 3-7 column volume The eluate was concentrated, added acetone to crystallize, separated, washed, and dried to obtain 22.7g of white powder pedigree H, which was detecte...

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Abstract

The invention relates to a preparation method of Ombuoside H, which is convenience for operation and has less pollution and energy consumption. The preparation method comprises the processing steps of: adding coarse pokeberry root in a CO2 supercritical extractor and obtaining an extract with n-butyl alcohol as an entrainer; adding the extract on a macroporous adsorption resin column for adsorption; eluting by ethanol; collecting the eluent; decompressing to recover the solvent and drying the solvent; adding the dried solvent onto a silica chromatographic column to elute by methanol-chloroform mixed solvent, wherein the proportion of the methanol to the chloroform in the mixed solvent is 1: 1; dividing and collecting the eluent according to column volume; combining eluent at the 3-7 partsof column volume for concentration; adding acetone crystal; and separating, washing and drying to obtain the Ombuoside H. By adopting the preparation method of the invention, the obtained Ombuoside Hhas high purity and the industrial enlargement is easy to realize.

Description

technical field [0001] The invention relates to a preparation method of pedicleside H, in particular to a preparation method of extracting pedicleside H from plants. Background technique [0002] Phytolaccasaponin H (Esculentoside H, Phytolaccasaponin B), molecular formula: C 48 h 76 o 21 , molecular weight: 989.116, CAS accession number: 66656-92-6. It mainly exists in a variety of plants of Phytolaraceae, among which Phytolacca acinosa Roxb. has a high content in the roots and rich sources of raw materials. Its molecular formula is as follows: [0003] [0004] Modern studies have shown that peduroside H has strong anti-tumor activity, and it is also used as a raw material for the synthesis of other active derivatives. [0005] The dried root of Phytolacca acinosa Roxb., a plant of Pokweed family, is used as a traditional Chinese medicine Phytolacca, which has the effects of dispelling water, reducing swelling, promoting diuresis, detoxifying and dispelling stagnat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00C07H15/256C07H1/08
CPCY02P20/54
Inventor 王峰王琳张发成
Owner SUZHOU PAITENG BIOLOGICAL MEDICAL TECH