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A high-efficiency and accurate method for separating and purifying deoxyterrain

A deoxo-rhein, separation and purification technology, which is applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve the problems affecting the physiological activity and efficacy of deoxo-rhein, and achieve a purification process. Perfect parameters, saving production cost and improving the effect of purity

Active Publication Date: 2015-12-02
KPC PHARM INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the Lhasa rhubarb extract of the prior art all contains other impurity components and similar structures, which has affected the physiological activity of deoxyrhein and the performance of the drug effect. How to find one or several stable crystal forms through crystallization to keep the target substance stable is very necessary for the clinical application of deoxyterretherin

Method used

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  • A high-efficiency and accurate method for separating and purifying deoxyterrain
  • A high-efficiency and accurate method for separating and purifying deoxyterrain
  • A high-efficiency and accurate method for separating and purifying deoxyterrain

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Preparation: crushed Lhasa rhubarb, sieve over 40 meters, and then add 1K Gg powder to add 1L ethanol to add 85%ethanol, extract 3 times in return, 2h each time, extract the solution merged and concentrateEssence

Embodiment 2

[0042] Take the Lhasa rhubarb extract, which is dissolved with a weap water with a weight of 1 times, and the aqueous solution is stirred and stirred to obtain the water solution.Wash the ionic water to colorless; then wash with the gradient of the alcohol solution: first washed with a low -concentration ethanol solution of 10%of the volume of 5 times the volume of 5 times the volume; then the medium -concentration ethanol solution of 5 times the volume of 5 times the volumeThe liquid is light yellow; finally uses a high-concentration ethanol solution of 6 times the volume of 6 times the volume of the volume to elute, collects the elution, condenses to the comparative density of 1.0 ~ 1.3 concentrated solution;Separate, wash with a 3x pillar volume to colorless; then use a high -concentration ethanol solution of 50%of the volume of 6 times the volume of 6 times the volume to elute, collect the elution liquid; condense the elux to the relative density 1.0 ~ 1.3 after 1.0 ~ 1.3, Col...

Embodiment 3

[0044] Take the Lhasa rhubarb extract, which is dissolved with a 3x weight removal water. After the aqueous solution is fully stirred, the centrifuge is separated to obtain the water liquid;6 times the size of the pillar volume was washed to colorless; then washed with a gradient of alcohol solution: first washed with a low concentration of low -concentration ethanol solution of 6 times the volume of 6 times the volume, and the medium -concentration ethanol solution of 80%of the volume of 6 times pillar was beforeWashing DC outflow is light yellow; 90%of the high concentration ethanol solution of 8 times the volume of 8 times pillar is eluted, collects the elution, concentrated to the relative density 1.0 ~ 1.3;Separate, wash with a 6x pillar volume to colorless; use 90%of the high concentration ethanol solution of 8 times the volume of 8 times pillar to elute and collect the elution liquid; condense the elux to relative density 1.0 ~ 1.3, cool down, cool down, cool down, cool dow...

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Abstract

The invention discloses a high-efficiency and accurate method for separating and purifying deoxyrheumin, comprising water extraction of extract, primary purification, secondary purification, roughing and refining. The crude product of deoxyreveredin is obtained, and the crude product is refined with water or low-carbon organic solvent and activated carbon to obtain high-purity deoxyrerbin in the form of light yellow fine grains. According to the physical and chemical characteristics of the extract from Lhasa rhubarb, the present invention adopts weak, medium and high polarity macroporous resin adsorption columns for multi-stage adsorption and separation, and stepwise washing and elution from low to high concentration ethanol solution, a single refining process can be obtained The high-quality deoxyrhein in the composition effectively removes other impurities, so that the purity of deoxyrhein can reach more than 98%. The invention overcomes the disadvantages of complex procedures and cumbersome operations in the prior art, effectively improves the purity of deoxyrhein, shortens the process time, saves production costs, improves the purification process parameters, and is beneficial to large-scale production.

Description

Technical field [0001] The present invention belongs to the field of Chinese medicine extraction technology, which involves a method of simplicity, stable and reliable technology, and accurately separate and purify the method of exfoliating and purifying the oxygen soil chloride. Background technique [0002] Deoxyrhaponticin is an effective ingredient to extract from Rheumlhasaensea.j.lietp.hsiaoinfl.xizang.1: 598.t.192: 1-3.1983).Lhasa Rhubarb is a plant of the rhodium of the Dahuang family."New Xiu Jingzhu Bencao" is listed as "sub -rhubarb" in Tibetan medicines, and its roots and rhizomes are used as medicine.Lhasa rhubarb is mainly produced in Tibet, Sichuan and other places in my country.The chemical composition of Lhasa rhubarb root stems has not been reported at present. Our preliminary research has found that there are multiple di -styrene compounds.Both belong to the pyramide compounds.The oxygen earth rhiline, its chemical structure is 5-hydroxyl-4'-methoxyl di-lymthyl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/203C07H1/08
Inventor 陈锦锌龚云麒方芳刘一丹
Owner KPC PHARM INC