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Method for purifying friedelin

A purification method, the technology of suberone, which is applied in the production of steroids, bulk chemicals, organic chemistry, etc., can solve the problems of difficulty in large-scale production, and achieve short cycle times, high product purity, and less solvent consumption Effect

Inactive Publication Date: 2012-07-04
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is only suitable for laboratory research and analysis, and is not easy for large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Pulverize Bamboo Ru, take 1kg and place it in an extraction tank, add 100ml of 95% ethanol solution, and carry out supercritical CO2 2 Extraction for 2h, extraction temperature was 45℃, extraction pressure was 40MPa, CO 2 The flow rate is 20L / h, the temperature of the separation kettle I is 40°C, the pressure is 6MPa, the temperature of the separation kettle II is 45°C, and the pressure is 6.5MPa, and 3L of 5% NaHCO is added to the extract. 3 solution, filter out the insoluble matter, suspend in water, extract with equal volume of chloroform, recover the solvent under reduced pressure in the chloroform layer, add 30 g of macroporous resin, mix the sample, evaporate the solvent, and install it on the top of the X-5 macroporous resin column. Elute with 3L of water, then successively use 3L of 30%, 3L of 50%, 3L of 70%, and 2L of 99% ethanol solution gradient elution to collect the eluent rich in cork ketone, concentrate and evaporate to dryness, use 200ml of ethyl acetate...

Embodiment 2

[0020] Pulverize Bamboo Ru, take 1kg and place it in an extraction tank, add 150ml of 95% ethanol solution, and carry out supercritical CO2 2 Extraction was carried out for 3 h, the extraction temperature was 60 °C, the extraction pressure was 35 MPa, CO 2 The flow rate was 25L / h, the temperature of the separation kettle I was 45°C, and the pressure was 8MPa, the temperature of the separation kettle II was 30°C, and the pressure was 5.5MPa, and 4L of 5% NaHCO was added to the extract. 3 solution, filter out the insolubles, suspend in water, extract with equal volume of chloroform, recover the solvent under reduced pressure in the chloroform layer, add 50 g of macroporous resin, mix the sample, evaporate the solvent, install it on the top of the D101 macroporous resin column, and use 4 L of water first. Elution, followed by gradient elution with 4L of 40%, 4L of 55%, 4L of 80%, and 3L of 95% ethanol solution, collected the eluent rich in cork, concentrated and evaporated to dry...

Embodiment 3

[0022] Pulverize Bamboo Ru, take 2kg and place it in an extraction tank, add 260ml of 95% ethanol solution, and carry out supercritical CO2 2 Extraction for 1 h, extraction temperature was 50 °C, extraction pressure was 25 MPa, CO 2 The flow rate was 30L / h, the temperature of the separation kettle I was 45 °C, and the pressure was 7MPa, the temperature of the separation kettle II was 35 °C, and the pressure was 4MPa, and the extract was added with 10L of 5% NaHCO. 3 solution, filter out the insoluble matter, suspend in water, extract with equal volume of chloroform, recover the solvent under reduced pressure in the chloroform layer, add 80 g of macroporous resin, mix the sample, evaporate the solvent, and install it on the top of the AB-8 macroporous resin column. Elution with 10L of water, followed by gradient elution with 6L of 40%, 6L of 60%, 6L of 80%, and 5L of 100% ethanol solution, collected the eluent rich in cork, concentrated and evaporated to dryness, dissolved in 3...

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Abstract

The invention provides a method for purifying friedelin, which is characterized by adopting supercritical carbon dioxide (CO2) extraction and macroporous resin purification friedelin. The method comprises the steps of extracting original medicinal material supercritical CO2, enabling extract to be soluble in sodium bicarbonate (NaHCO3) solution, filtering out insoluble substance, mixing and suspending on water, extracting by using trichloromethane, obtaining a trichloromethane layer for reducing pressure and recovering solvent, enabling the ethanol to be dissolved, adding defined amount macroporous resin to be evenly mixed, drying the solvent in a waving mode, conducting gradient elute on the water and ethanol solution in different concentration, collecting the eluent being rich in the friedelin, concentrating and drying backflow solution of ethyl acetate, stewing and crystallizing, filtering out crystallization and drying to obtain products. The method for purifying the friedelin is simple in step, good in selected separating effect, high in extraction efficiency and capable of being popularized and conducting large-scale production.

Description

Technical field: [0001] The invention belongs to the technical field of natural medicine extraction, and relates to a method for extracting and purifying cork ketone by applying a supercritical extraction method and a macroporous resin method. Background technique: [0002] Bamboo ru is the outer cortex or the next layer scraped by the stems of some bamboo species in the genus Poaceae, Pseudomonas spp. and Pseudomonas spp. It is used for cough with phlegm heat, gallbladder fire with phlegm, vomiting with vexed heat, palpitation and insomnia, stroke, phlegm confusion, tongue strength and muteness, stomach heat and vomiting, dysentery of pregnancy, disturbed fetal movement, etc. [0003] Corkone, corkane-type pentacyclic triterpenoid, needle crystal, melting point 263-263.5℃, soluble in chloroform, petroleum ether and hot ethanol, insoluble in water. Corylinone exists in many plants, such as the whole grass of Euonymus euphorbia, the stem of Euphorbiaceae, the stem of Euphorb...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
CPCY02P20/54
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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