Purification method of rhubarb stilbene glucoside

A purification method and technology of tristilbene, which is applied in the field of compound extraction and purification, can solve the problems of small sample processing volume, unable to obtain ideal purity of tristilbene, polluting the environment, etc.

Active Publication Date: 2012-09-12
KPC PHARM INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Applying a large amount of organic solvents to industrial production is not conducive to the control of production conditions, especially chloroform is a solvent with low boiling point and high toxicity, which not only affects the personal safety of operators, but also pollutes the environment
At the same time, considering that the silica gel column is usually difficult to regenerate, the amount of sample processing is relatively small, and the current purification technology cannot obtain tristilbene with ideal purity, therefore, a purification method that can obtain tristilbene with higher purity is provided , is of great significance

Method used

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  • Purification method of rhubarb stilbene glucoside
  • Purification method of rhubarb stilbene glucoside
  • Purification method of rhubarb stilbene glucoside

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Take 2000g of Lhasa rhubarb crude powder, extract with 16L of 95% ethanol under reflux for 3 times, 2 hours each time, filter, combine the filtrates, concentrate to dryness under reduced pressure, add 2000ml of water to the residue and stir to dissolve. Sampling for HPLC detection, see figure 1 .

[0042]Measure 1600ml of the supernatant of the medicinal liquid, load the sample onto D101 macroporous adsorption resin, wash 5-6 times the column volume with water, then flush the column with 25%-30% ethanol aqueous solution, collect 2-6 times the volume of the effluent, After mixing, samples were taken for HPLC detection. See figure 2 . The remaining solution was concentrated under reduced pressure to remove ethanol to obtain about 1400 ml of an aqueous solution.

[0043] Take 200ml of the remaining aqueous solution, select different types of resins for secondary loading, and elute with 90% ethanol, collect 5 times the column volume of ethanol solution, concentrate to ...

Embodiment 2

[0066] Take 2000g of Lhasa rhubarb crude powder, extract with 16L of 95% acetone under reflux for 3 times, 2 hours each time, filter, combine the filtrates, concentrate to dryness under reduced pressure, add 2000ml of water to the residue and stir to dissolve. Let stand for 24 hours. Take the supernatant liquid for later use. Samples were taken for HPLC detection.

[0067] Measure 1600ml of the supernatant of the medicinal liquid, load the sample onto D101 macroporous adsorption resin, wash 5-6 times the column volume with water, then flush the column with 25%-30% ethanol aqueous solution, collect 2-6 times the volume of the effluent, After mixing, samples were taken for HPLC detection. The remaining solution was concentrated under reduced pressure to remove ethanol to obtain about 1400 ml of an aqueous solution.

[0068] Take 200ml of the remaining aqueous solution, select HPD-500 for secondary loading, elute with 90% ethanol, collect 5 times the column volume of ethanol s...

Embodiment 3

[0088] Take 2000g of Lhasa rhubarb crude powder, reflux extraction with 16L of 95% methanol for 3 times, 2 hours each time, filter, combine the filtrates, concentrate to dryness under reduced pressure, add 2000ml of water to the residue and stir to dissolve. Let stand for 24 hours. Take the supernatant liquid for later use. Samples were taken for HPLC detection.

[0089] Measure 1600ml of the supernatant of the medicinal liquid, load the sample onto D101 macroporous adsorption resin, wash 5-6 times the column volume with water, then flush the column with 25%-30% ethanol aqueous solution, collect 2-6 times the volume of the effluent, After mixing, samples were taken for HPLC detection. The remaining solution was concentrated under reduced pressure to remove ethanol to obtain about 1400 ml of an aqueous solution.

[0090] Take 200ml of the remaining aqueous solution, use ADS-17 for secondary loading, elute with 90% ethanol, collect 5 times the column volume of ethanol solutio...

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Abstract

The invention relates to the field of compound extraction and purification, in particular to a purification method of rhubarb stilbene glucoside. The purification method comprises the following steps: taking rheum lhasaense, extracting with ethanol and carrying out non-polar macro-porous resin first purification; eluting with ethanol water solution, collecting a first eluent and carrying out polar resin or non-polar resin second purification of a styrene framework structure; and eluting with ethanol water solution with a concentration of 80-95 percent, collecting a second eluent and refining. The method has the advantages of simplicity and convenience in operation, easiness in reproduction, shortened purification and reduced energy consumption, and the purity of rhubarb stilbene glucoside reaches above 98 percent.

Description

technical field [0001] The invention relates to the field of compound extraction and purification, in particular to a method for purifying tristilbene. Background technique [0002] The chemical structure of trihydroxy-stilbene-3'-b-D-glucosides (3,5,3',4'-trihydroxy-stilbene-3'b-D -glucoside), molecular formula C20H22O9; molecular weight 406.13, structure as shown in formula I: [0003] [0004] Formula I [0005] Tristilbene glycoside is easily soluble in methanol, ethanol, hot water, sodium bicarbonate and sodium hydroxide aqueous solution, soluble in ethyl acetate, slightly soluble in cold water, and hardly soluble in ether. [0006] Trizastilbene is an active ingredient extracted from the rhizome of the medicinal material Lhasa Rhubarb. Rheum lhasaense A.J.Li et P.K.Hsiao is a plant of the wave leaf group of Rhubarb. It is a herbal medicine used by Tibetan folks. It is called Quzha in Tibetan. In "Xinxiu Jingzhu Materia Medica", it is listed as "sub-rhubarb" in T...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/203C07H1/08
Inventor 陈锦锌龚云麒方芳
Owner KPC PHARM INC
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