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Method for separating and preparing ursolic acid methyl ester from dracocephalum heterophyllum benth and application of ursolic acid methyl ester

A technology of ursyl methyl ester and isophyllum is applied in the field of preparation of natural active ingredients, can solve problems such as the preparation and active application of ursine methyl ester monomers, and achieve good pharmacological activity, high separation efficiency, and high separation purity. Effect

Inactive Publication Date: 2014-11-19
CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Relevant literatures at home and abroad show that there is no relevant report on the preparation and active application of urethane methyl ester monomer so far

Method used

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  • Method for separating and preparing ursolic acid methyl ester from dracocephalum heterophyllum benth and application of ursolic acid methyl ester
  • Method for separating and preparing ursolic acid methyl ester from dracocephalum heterophyllum benth and application of ursolic acid methyl ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1 The method for isolating and preparing ursyl methyl from the different leaf green orchids, comprises the following steps:

[0045] ⑴Cut 1 kg of Cymbidium isophyllum into 2cm sections, then add ethanol with a mass concentration of 90% according to the mass volume ratio of 1 kg:12 L, and carry out reflux extraction at a temperature of 70°C, and the extraction times are 2 times, 2 hours each time, combined to obtain the extract; the extract was concentrated under reduced pressure at a temperature of 65° C. and a vacuum of 0.7 MPa to obtain the extract.

[0046] (2) The extract was extracted with ethyl acetate at room temperature according to the mass-volume ratio of 1 kg: 1.5 L. The extraction times were 3 times, 2 hours each time, and combined to obtain the extract. The extract was stored at a temperature of 45°C, Concentrate under reduced pressure under the condition of vacuum degree of 0.7MPa to obtain the crude extract of methyl ursate.

[0047] (3) Di...

Embodiment 2

[0050] Example 2 The method for isolating and preparing ursyl methyl from the different leaf green orchids, comprises the following steps:

[0051] ⑴Cut 2 kg of Cymbidium heterophyllum into 1 cm sections, then add ethanol with a mass concentration of 85% according to the mass volume ratio of 1 kg: 9 L, and carry out reflux extraction at a temperature of 65 °C, and the extraction times are 2 times, 1 hour each time, combined to obtain the extract; the extract was concentrated under reduced pressure at a temperature of 60° C. and a vacuum of 0.6 MPa to obtain the extract.

[0052] (2) The extract was extracted with ethyl acetate at room temperature according to the mass-volume ratio of 1 kg: 1 L, and the number of extractions was 3 times, each time for 2 hours. Concentrate under reduced pressure under the condition of vacuum degree of 0.6 MPa to obtain the crude extract of methyl ursate.

[0053] (3) Dissolve the crude extract of methyl urethane in ethyl acetate, then add...

Embodiment 3

[0056] Example 3 The method for isolating and preparing ursyl methyl from the different leaf green orchids, comprises the following steps:

[0057] ⑴Cut 3kg of Cymbidium heterophylla into 3cm sections, then add ethanol with a mass concentration of 95% according to the mass volume ratio of 1 kg: 15 L, and carry out reflux extraction at a temperature of 75°C, and the extraction times are 3 times, 3 hours each time, combined to obtain the extract; the extract was concentrated under reduced pressure at a temperature of 70°C and a vacuum of 0.8 MPa to obtain the extract.

[0058] (2) The extract is extracted with ethyl acetate at room temperature according to the mass volume ratio of 1 kg: 2 L. The extraction times are 3 times, each time 2 hours, and the extract is combined to obtain the extract. The extract is stored at a temperature of 50 ° C, Concentrate under reduced pressure under the condition of vacuum degree of 0.8 MPa to obtain the crude extract of methyl-usuate.

...

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Abstract

The invention relates to a method for separating and preparing ursolic acid methyl ester from dracocephalum heterophyllum benth. The method comprises steps as follows: (1), dracocephalum heterophyllum benth is cut into sections and subjected to reflux extraction by ethyl alcohol to obtain an extracting solution; and the extracting solution is concentrated under reduced pressure to obtain extracts; (2), the extracts are extracted by ethyl acetate under the ambient temperature condition to obtain an extract liquid, and the extract liquid is concentrated under reduced pressure to obtain crude extracts of ursolic acid methyl ester; (3), the crude extracts of ursolic acid methyl ester are dissolved in ethyl acetate, silica gel is added, the mixture is stirred and mixed, silica gel columns are fed with a dry method twice after the solvent of ethyl acetate volatilizes, and purer ursolic acid methyl ester is obtained after concentration under reduced pressure; and (4), the purer ursolic acid methyl ester is dissolved and crystallized for impurity removal and then filtered to obtain ursolic acid methyl ester crystals. The method is simple, simple and convenient to operate and high in separation efficiency and separation purity; and meanwhile, the ursolic acid methyl ester crystals obtained with the method can be applied to treatment of tumor and acute liver injury diseases.

Description

technical field [0001] The present invention relates to a preparation method and application of a natural active ingredient, in particular to a method for separating and preparing ursyl methyl from Cyperus heterophylla and its application. Background technique [0002] different leaf green orchid ( Dracocephalum heterophyllum Benth.) It is a herbaceous plant of the genus Qinglan of the Labiatae, also known as Baihua Zhizihua, Baihua Prunella, Jizi Qingbao (Tibetan medicine name), and Xinjiang Uyghur language called Marzan Juxi and Zupar. The aerial part of the different leaf green orchid has the function of calming the liver and clearing away heat. Its smell is sweet and moist, and it smells refreshing. It is a traditional medicine used by the Uighurs and Tibetans to treat cough, asthma and stomach problems. It is mainly used to treat jaundice fever, Liver fever, febrile venereal headache, ophthalmopathy, oral ulcers, bronchitis, high blood pressure and other diseases. In ...

Claims

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Application Information

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IPC IPC(8): C07J63/00A61K31/56A61P35/00A61P1/16
Inventor 岳会兰赵晓辉邵赟梅丽娟王启兰陶燕铎
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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