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Separation method of madecassic acid compound

A technology for the separation of madecassic acid and its separation method, which is applied in the field of separation of madecassic acid compounds, and can solve problems such as contamination of absorption pools, blockage of liquid chromatography channels, and impact on the service life of chromatographic columns, so as to improve separation efficiency and use The effect of long life and low cost of solvent

Active Publication Date: 2018-12-07
SHANGHAI INST OF PHARMA IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem solved by the present invention is to overcome the prior art in the prior art of hydroxyasiatic acid and asiatic acid B using reverse phase C in high performance liquid chromatography. 18 When the chromatographic separation is performed, the β-cyclodextrin in the mobile phase affects the service life of the chromatographic column, and may easily cause problems such as liquid chromatographic channel blockage and contamination of the absorption pool, thus providing a separation method of madecassic acid and asiatic acid B method

Method used

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  • Separation method of madecassic acid compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weighing the mixture sample containing madecassic acid and asiatic acid B to be separated, adding methanol and ultrasonically dissolving to prepare a solution containing about 0.5-1 mg of the sample to be separated per milliliter.

[0025] The above solution is used as the sample to be tested, and the injection volume is 5ul: refer to the following conditions for analysis and detection,

[0026] Analytical supercritical fluid chromatography (Agilent SFC-D) was equipped with a UV detector, and an analytical cellulose chromatographic column (Pheno Lux Cellulose-2, 150×4.6mm I.D., 3 μm) was selected, and the mobile phase was carbon dioxide-methanol (containing 0.05% diethylamine) (60:40), flow rate 2.5mL / min, pressure 100bar, column temperature 35°C, detection wavelength 210nm.

[0027] The results of SFC analysis showed that: madecassic acid and asiatic acid B in the sample can be separated well, the separation time is 3.058min and 2.445min respectively, and the separatio...

Embodiment 2

[0029] Mobile phase is carbon dioxide-ethanol (containing 0.05% diethylamine), and all the other operations are with embodiment 1,

[0030] The results of SFC analysis showed that: madecassic acid and asiatic acid B in the sample can be separated well, the separation time is 2.66min and 2.29min respectively, and the separation degree is greater than 1.5.

Embodiment 3

[0032] The chromatographic column is CHIRALPAK IC-3, and the rest of the operations are the same as in Example 1.

[0033] SFC analysis results showed that: madecassic acid and asiatic acid B in the sample could be separated well, the separation time was 5.35min and 5.07min respectively, and the separation degree was greater than 1.5.

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Abstract

The invention discloses a separation method of a madecassic acid compound. According to the separation method, separation is carried out by adopting a supercritical fluid chromatograph, and a cellulose chiral column is adopted as a chromatographic column. The separation effect of the method is good, the purity of a separated product is high, the separation speed is high, meanwhile, the service life of the chromatographic column is long, a solvent is low in cost, is free of pollution, and can be recycled, the separation efficiency is greatly improved, and the production cost is reduced.

Description

technical field [0001] The invention relates to a separation method of madecassic acid compounds. Background technique [0002] Madecassic acid (as shown in formula 1) and asiatic acid B (as shown in formula 2) are madecassic acid compounds, the two are isomers, and the molecular formula is C 30 h 48 o 6 (molecular weight is 504), its chemical structural formula is as follows: [0003] [0004] As a pentacyclic triterpenoid compound, madecasic acid mainly exists in the form of glycosides or free aglycones in the Umbelliferae plant Centella asiatica, and has the functions of promoting wound healing and inhibiting scar hyperplasia. In recent years, there have been research reports on anti-tumor and anti-fibrosis and related patent applications. For example, the Chinese patent application CN201410046878.9 entitled "A kind of madecassate and its preparation method and use" records that madecassic acid is The active metabolized form of its glycosides in the gastrointestina...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00C07B63/00
CPCC07B63/00C07B2200/09C07J63/008Y02P20/54
Inventor 徐云辉刘灿灿华茉莉刘洁苏晓丽
Owner SHANGHAI INST OF PHARMA IND CO LTD
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