Separation and purification method of pachymic acid monomer

A technology for separation and purification of tacosic acid, applied in chemical recovery, organic chemistry, steroids, etc., can solve the problems of inability to industrialize production, high preparation cost, complicated process, etc., and achieve cost saving of reagents, easy operation and high product purity. Effect

Active Publication Date: 2014-03-26
CHENGDU PUSH BIOLOGICAL TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0007] The present invention aims to overcome the disadvantages of complex process, high preparation cost, long cycle and im

Method used

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  • Separation and purification method of pachymic acid monomer

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Embodiment 1

[0035] A. Extraction

[0036] Grind 250 g of Poria cocos into coarse powder, add 2.0 L of ethanol solution with a mass percentage concentration of 95%, reflux extraction 3 times, each time for 1.5 hours, filter the extract, combine the filtrate, concentrate under reduced pressure to recover ethanol, and obtain a concentrated extract The relative density is 1.32 (50°C), and the volume is 160ml;

[0037] B. Extraction

[0038] Add 1.6L of water to the concentrated extract obtained in step A to disperse, extract 3 times with petroleum ether, remove the petroleum ether extract, extract the aqueous phase 5 times with ethyl acetate, combine the ethyl acetate extract, reclaim the filtrate to dryness, and obtain Off-white pachymic acid crude product 1.4g;

[0039] C. crystallization

[0040] Completely dissolve the off-white solid obtained in step B with 140ml of acetone, filter it with a nano-organic membrane, add 280ml of distilled water to the filtrate, refrigerate and crystalli...

Embodiment 2

[0042] A. Extraction

[0043] Grind 250 g of Poria cocos into coarse powder, add 2.5 L of ethanol solution with a mass percentage concentration of 95%, reflux extraction 4 times, each time for 2 hours, filter the extract, combine the filtrate, concentrate under reduced pressure to recover ethanol, and obtain a concentrated extract The relative density is 1.35 (50°C), and the volume is 120ml;

[0044] B. Extraction

[0045] Add 1.2 L of water to the concentrated extract obtained in step A to disperse, extract 3 times with petroleum ether, remove the petroleum ether extract, extract the aqueous phase with ethyl acetate 6 times, combine the ethyl acetate extract, and recover the filtrate to dryness to obtain Off-white pachymic acid crude product 1.55g;

[0046] C. crystallization

[0047] Completely dissolve the off-white solid obtained in step B with 310ml of acetone, filter it with a nano-organic membrane, add 930ml of distilled water to the filtrate for refrigeration and cr...

Embodiment 3

[0049] A. Extraction

[0050] Grind 250 g of Poria cocos into coarse powder, add 2.5 L of ethanol solution with a mass percentage concentration of 95%, reflux extraction 3 times, each time for 2 hours, filter the extract, combine the filtrate, concentrate under reduced pressure to recover ethanol, and obtain a concentrated extract The relative density is 1.30 (50°C), and the volume is 130ml;

[0051] B. Extraction

[0052]Add 1.3 L of water to the concentrated extract obtained in step A to disperse, extract 4 times with petroleum ether, remove the petroleum ether extract, extract the aqueous phase with ethyl acetate 4 times, combine the ethyl acetate extract, reclaim the filtrate to dryness, and obtain Off-white pachymic acid crude product 1.3g;

[0053] C. crystallization

[0054] Completely dissolve the off-white solid obtained in step B with 390ml of acetone, filter it with a nano-organic membrane after dissolution, add 1460ml of distilled water to the filtrate for refri...

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Abstract

The invention relates to a separation and purification method of a pachymic acid monomer, and belongs to the technical field of separation and purification of active ingredients of traditional Chinese medicines. The pachymic acid monomer is obtained by taking poria cocos as a raw material, extracting twice and crystallizing. The method specifically comprises the following main steps: A, extracting, namely grinding the poria cocos into coarse powder, and performing reflux extraction by ethanol to obtain thick extractum; B, extracting, namely extracting the thick extractum by ethyl acetate to obtain a crude product of pachymic acid; C, crystallizing, namely dissolving the crude product by an organic solvent, crystallizing and filtering to obtain the pachymic acid monomer with the purity not less than 98%. The whole process is easy and convenient to operate, stable, low in cost, high in separation efficiency and product purity, and suitable for the industrialization production of the high-purity pachymic acid monomer.

Description

technical field [0001] The invention relates to a method for separating and purifying active components of traditional Chinese medicines, in particular to a method for extracting and separating pachymic acid monomers from poria cocos, and belongs to the technical field of separation and purification of traditional Chinese medicines. Background technique [0002] The English name of Pachymic acid is Pachymic acid, CAS: 29070-92-6, and the molecular formula is C 33 h 52 o 5 , the molecular weight is 528.76, and the structural formula is as follows: [0003] [0004] A recent research report pointed out that Poria cocos extract has an effect on the concentration of calcium ions in the central cranial nerve. Poria cocos is clinically used in schizophrenia, anti-tumor, edema, infantile diarrhea, dizziness, etc. These are consistent with the theory of traditional Chinese medicine that invigorates the spleen, replenishes vital energy and enhances immunity. However, foreign s...

Claims

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Application Information

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IPC IPC(8): C07J9/00
CPCY02P20/582
Inventor 李启发文焕松陈军刘丁
Owner CHENGDU PUSH BIOLOGICAL TECH
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