Preparation method of oleanolic acid

A technology of oleanolic acid and microfiltration is applied in the field of preparation of oleanolic acid, which can solve the problems of large dosage, low extraction selectivity, large consumption of solvent and the like

Inactive Publication Date: 2010-07-07
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In the prior art, the extraction and separation method of oleanolic acid mainly adopts solvent extraction method, etc., but this method needs to consume a large amount of solvent, and when using some organic solvents, it will also cause solvent residue, the selectivity of extraction is not high, and the production The dosage forms of the medicines obtained are relatively single, mostly decoctions, pills, powders, etc., and the dosage is large and inconvenient to carry

Method used

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  • Preparation method of oleanolic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Take 10 kg of fresh Ligustrum lucidum leaves (1.2% oleanolic acid content), add 100 L of supersaturated lime water, decoct for 2 hours, add 100 L of supersaturated lime water to the filtered insoluble matter, decoct for 2 hours, and filter. Combine the two medicinal solutions, add hydrochloric acid, adjust the pH to about 3, and filter with suction to obtain 218 g of the precipitated crude triterpene acid. Add 900ml of 50% methanol for reflux extraction for 1.5 hours, filter while hot, and filter the filtrate through a ceramic membrane with a pore size of 50-500nm, and then through a nanofiltration membrane with a molecular weight cutoff of 300-500, and dry under reduced pressure to obtain 93g of oleanolic acid. The purity was 98.5%.

Embodiment 2

[0021] Take 10kg of fresh Ligustrum lucid leaves (1.2% oleanolic acid content), add 110L of supersaturated lime water, decoct for 2.5 hours, add supersaturated lime water to the filtered insoluble matter, and operate twice under the same conditions. Combine the three liquid medicines, add sulfuric acid, adjust the pH to about 3, and filter with suction to obtain 223 g of the precipitated crude triterpene acid. Add 1000ml of 55% methanol for reflux extraction for 2 hours, filter while hot, and filter the filtrate through a ceramic membrane with a pore size of 50-500nm, and then through a nanofiltration membrane with a molecular weight cut-off of 300-500. Dry under reduced pressure to obtain 107g of oleanolic acid. The purity was 98.2%.

Embodiment 3

[0023] Take 10kg of fresh Ligustrum lucid leaves (with oleanolic acid content 1.1%), add 110L of supersaturated lime water, decoct for 3 hours, add supersaturated lime water to the filtered insoluble matter, and operate once under the same conditions. Combine the two medicinal solutions, add phosphoric acid, adjust the pH to about 2, and filter with suction to obtain 213 g of the precipitated crude triterpene acid. Add 900ml of 60% methanol for reflux extraction for 1.5 hours, filter while hot, and filter the filtrate through a ceramic membrane with a pore size of 50-500nm, and then through a nanofiltration membrane with a molecular weight cutoff of 300-500, and dry under reduced pressure to obtain 96g of oleanolic acid. The purity was 98.5%.

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Abstract

The invention relates to a preparation method of oleanolic acid. In the process, glossy privet fruit is taken as the raw material, a crude product is obtained through extraction for 2-3 times by oversaturated lime water with 2-3 hours for each time, liquid medicine combination, acidification by adding acid and filtration; backflow extraction is carried out on the crude product by 50-60% of methanol; and the product can be obtained through heated filtration, microfiltration and impurity removing of the filtrate, nanofiltration, concentration and drying. The process has the advantages of simple and convenient operation, little pollution and less equipment investment and is beneficial for large-scale operation.

Description

Technical field [0001] The invention relates to a method for preparing oleanolic acid, in particular to a method for extracting oleanolic acid from Ligustrum lucidum. Background technique [0002] Ligustrum lucidum is the dried and mature fruit of Ligustrum Lucidumt, a plant of the oleaceae family. It is a commonly used Chinese medicine and the main component of many kinds of patent medicines and prescriptions. The main ingredient is oleanolic acid. [0003] Oleanolic acid (Oleanolic acid, OA), also known as qingsisu, is a chemical component of natural products, widely present in oldenlandia diffusa, hawthorn, clove, jujube, ligustrum lucidum in free or combined form of glycosides , Loquat leaves, oak, prunella vulgaris and other plants. Five ring triterpenoids, the chemical name is (3β)-3-Hydroxyolean-12-en-28-oic acid. Molecular formula: C 30 H 48 O 3 , Molecular weight: 456.707, white crystalline powder, odorless, tasteless, insoluble in water, soluble in methanol, ethanol, b...

Claims

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Application Information

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