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Method for preparing pomolic acid

A technology of pom alkyd and ethanol, which is applied in the field of preparation of pom alkyd, can solve the problems that there are no reports on the technology of pom alkyd, and achieve the effects of avoiding adverse effects, mild conditions and reasonable process

Inactive Publication Date: 2013-12-25
NANJING TONGZE AGRI SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the prior art, there is no process report suitable for preparing pampol acid in large quantities

Method used

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  • Method for preparing pomolic acid

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Effect test

Embodiment 1

[0018] Pulverize the root medicinal material of Burnet, take 5kg and put it into a supercritical extraction tank, add an ethanol solution with a volume percentage of 80% as an entrainer, the addition amount is 0.3kg (6% of the weight of the raw material), and the extraction pressure is 25MPa, and the extraction temperature is 45°C, CO 2 Extract for 2 hours at a flow rate of 18L / h to obtain the root extract of Burnet elata. The extract is dispersed in hot water and put on a polyamide resin column at a flow rate of 1.0BV / h. Elution, finally eluted with 80% ethanol, collected 80% ethanol eluate, concentrated the eluate under reduced pressure to a relative density of 1.08, to obtain the crude extract of plamulol acid, the crude extract of plamulol acid was used Dissolved in methanol, mixed with 3 times the amount of acidic alumina, dried at 50°C at low temperature, put on the column by dry method, eluted with ethyl acetate-ethanol (1:2) and ethanol in sequence, checked by thin lay...

Embodiment 2

[0020] Pulverize the root medicinal material of Burnet, take 5kg and put it into a supercritical extraction tank, add a 70% ethanol solution as an entrainer in an amount of 0.6kg (12% of the weight of the raw material), at an extraction pressure of 20MPa, an extraction temperature of 35°C, CO 2 Extract for 1 hour at a flow rate of 20L / h to obtain the root extract of Burnet elata. The extract is dispersed in hot water and put on a polyamide resin column at a flow rate of 1.5BV / h. Elution, finally eluted with 90% ethanol, collected 90% ethanol eluate, concentrated the eluate under reduced pressure to a relative density of 1.10, to obtain the crude extract of plamulol acid, the crude extract of plamulol acid was used Dissolved in methanol, mixed with 3 times the amount of acidic alumina, dried at 45°C at low temperature, put on the column by dry method, eluted with ethyl acetate-ethanol (1:2) and ethanol in sequence, and checked by thin layer chromatography. The fractions with h...

Embodiment 3

[0022] Pulverize the root medicinal material of Burnet, take 5kg and put it into a supercritical extraction tank, add acetone solution with a volume percentage of 90% as an entrainer, the amount added is 0.75kg (15% of the weight of the raw material), and the extraction pressure is 32MPa, and the extraction temperature is 30°C, CO 2 Extract for 3 hours under the condition of a flow rate of 10L / h to obtain the root extract of Burnet. The extract is dispersed in hot water and put on a polyamide resin column at a flow rate of 1.2BV / h. Elution, finally eluted with 70% ethanol, collected 70% ethanol eluate, concentrated the eluate under reduced pressure to a relative density of 1.12, and obtained the crude extract of pomulol acid, used Dissolved in methanol, mixed with 3 times the amount of acidic alumina, dried at 40°C at low temperature, put on the column by dry method, eluted with ethyl acetate-ethanol (1:2) and ethanol in turn, checked by thin layer chromatography, collected T...

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Abstract

The invention discloses a method for preparing pomolic acid. The method is characterized by comprising the following steps of supercritical extraction, polyamide column chromatography, alumina column chromatography, recrystallizing and the like. The method is mild in conditions, an adverse effect of local high temperature on the product activity in the traditional method is avoided, the process is reasonable, rapid extraction, separation and purification can be realized, and the method is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of natural medicines, and in particular relates to a preparation method of pomulol acid. Background technique [0002] Pomolic acid is a triterpenoid compound isolated from the root of Sanguisorba officinalis L., Labiatae. It is a colorless needle crystal, mp.293-295℃, molecular weight 472.71, molecular formula C 30 h 48 o 4 , the structural formula is: [0003] [0004] Pharmacological studies have shown that pomerol acid has cytotoxic activity, and its ED50 against P388 is 2.9 μg / mL; it has antibacterial effect, and its MICs against Staphylococcus aureus, Streptococcus mutans and Pseudomonas aeruginosa are 25 μg / mL, 12.5~ 25μg / mL, 25μg / mL. [0005] In the prior art, there is no process report suitable for the large-scale preparation of pomulokic acid. Contents of the invention [0006] The object of the present invention is to provide a kind of preparation method of pomulak acid, adopt supercritical CO 2...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
CPCY02P20/54
Inventor 杨存
Owner NANJING TONGZE AGRI SCI & TECH
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