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Method for preparing high-purity oleanolic acid from Aralia taibaiensis

A technology of oleanolic acid and Aralia, applied in the directions of steroids, organic chemistry, etc., can solve the problems of long preparation cycle and high cost, and achieve the effects of reducing consumption cost, less waste, and short separation time

Inactive Publication Date: 2014-09-10
陕西医药控股集团新药技术开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation cycle is long and the cost is high. Based on the above reasons, the development of new separation and purification processes and the search for more economical, efficient and fast separation and purification technologies have increasingly become the focus of researchers.

Method used

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  • Method for preparing high-purity oleanolic acid from Aralia taibaiensis
  • Method for preparing high-purity oleanolic acid from Aralia taibaiensis

Examples

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Embodiment 1

[0042] A method for separating high-purity oleanolic acid from Aralia taibai, comprising the following steps:

[0043] 1) Take 1Kg of the dried rhizome of Aralia taibai, wash it with water, dry it, and crush it; add it to 10L water and boil for 1.5 hours, pour off the boiling liquid, and extract the dregs with 95% ethanol in 3 times of reflux, and the amount of ethanol used each time 6L;

[0044] 2) Combine the alcohol extract and 0.3% of the volume of the alcohol extract with activated carbon, stir and decolorize at 50°C for 1 hour; filter the activated carbon, and use 1.0mol / L sodium hydroxide aqueous solution to adjust the pH value of the ethanol extract to 11 After standing for 12 hours, filter to remove precipitates and filter impurities, and then concentrate the filtrate under reduced pressure to about 1 / 3 (5L) of the volume before concentration at 40°C with a vacuum of 0.15Mpa, and a large amount of insoluble matter is precipitated , filtered, and the insolubles filter...

Embodiment 2

[0049] A method for separating high-purity oleanolic acid from Aralia taibai, comprising the following steps:

[0050] 1) Take 1Kg of the dried rhizome of Aralia taibai, wash it with water, dry it, and crush it; add it to 12L water and boil for 1.0 hour, pour off the boiling liquid, and extract the dregs with 90% ethanol in 3 times of reflux, and the amount of ethanol used each time 8L;

[0051] 2) Combine the alcohol extract and the activated carbon with 0.6% volume of the alcohol extract, stir and decolorize at 60°C for 0.8 hours; filter the activated carbon, and adjust the pH value of the ethanol extract to 11 for the decolorized alcohol extract with 0.6mol / L sodium hydroxide aqueous solution After standing still for 10 hours, filter to remove precipitates and filter impurities, and concentrate the filtrate under reduced pressure to about 1 / 4 (6L) of the volume before concentration at 55°C with a vacuum degree of 0.12Mpa, and a large amount of insoluble matter precipitates ...

Embodiment 3

[0056] A method for separating high-purity oleanolic acid from Aralia taibai, comprising the following steps:

[0057] 1) Take 1Kg of the dried rhizome of Aralia taibai, wash it with water, dry it, and crush it; add it to 15L of water and boil for 2.0 hours, pour off the boiling liquid, and extract the dregs with 85% ethanol in 3 times of reflux, and the amount of ethanol used each time 12L;

[0058] 2) Combine the alcohol extract and the activated carbon with 1.0% volume of the alcohol extract, stir and decolorize at 55°C for 0.6 hours; filter the activated carbon, and use 0.8mol / L sodium hydroxide aqueous solution to adjust the pH value of the ethanol extract to 11 After standing for 8 hours, filter, remove precipitates, filter impurities, and concentrate the filtrate under reduced pressure to about 1 / 5 (7L) of the volume before concentration at 60°C with a vacuum degree of 0.09Mpa, and a large amount of insoluble matter is precipitated , filter, filter out insoluble matter...

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Abstract

The invention discloses a method for preparing high-purity oleanolic acid from Aralia taibaiensis, belonging to the technical field of natural product extraction separation. The method comprises the following steps: 1) washing an Aralia taibaiensis oleanolic acid crude product with water, taking the insoluble substance, adding analytic methanol into the insoluble substance, sufficiently and evenly mixing, filtering, and taking the supernatant to obtain a loading solution; 2) filling a high-pressure preparative liquid chromatography column with octadecylsilane bonded silica gel, loading the loading solution to the high-pressure preparative liquid chromatography column, and eluting by using a methanol-water system as an eluate; and 3) carrying out sectional collection under the detection of an ultraviolet detector to obtain an oleanolic acid solution, concentrating the oleanolic acid solution under reduced pressure, and washing with water to obtain the high-purity oleanolic acid. The method can be used for directly and quickly separating out the oleanolic acid, and has the advantages of short separation time and high separation quantity; the yield is up to 85% above, and the purity is up to 98% above; and the method has the characteristics of less generated waste, small required eluate volume, recyclable filler and solvent and environment friendliness, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of extraction and separation of natural products, and in particular relates to a method for separating and extracting oleanolic acid from Aralia taibai. Background technique [0002] Aralia taibai, also known as flying centipede seven, is a perennial plant of the Araliaceae genus. It is distributed in the western region of my country and has very rich wild resources. Taibai Aralia is also known as Aralia alba, which is recorded in the Chinese Medicine Dictionary as Aralia alba. This medicinal material has the effects of invigorating the stomach, astringent, diuresis and sugar production, and can nourish the waist and kidneys, strengthen the muscles and bones, relax the body and activate blood circulation, etc. [0003] Oleanolic acid, clinically used in the treatment of infectious acute jaundice hepatitis, has obvious effects of reducing alanine aminotransferase and jaundice, improving symptoms, signs and l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
Inventor 肖志强杨建刚朱爱华郭晨史文静任哲张俏张建辉
Owner 陕西医药控股集团新药技术开发有限公司
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