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Purification method of madecassoside

A technology of madecassoside and a purification method, which is applied in the field of purification of madecassoside, can solve the problems of inapplicability to industrialized production, large amount of solvent used, and high production cost, and achieve low production cost, high product yield and high production cost. The effect of high purity and low requirements for equipment

Pending Publication Date: 2021-12-17
INCREASEPHARM TIANJIN INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the existing reports, the purification process of madecassoside mainly includes: through the preparative high performance liquid chromatography analysis method, using cyclodextrin as the mobile phase additive method for separation, the disadvantages are: the use of a large amount of solvent, the production cost High, not suitable for future industrial production

Method used

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  • Purification method of madecassoside
  • Purification method of madecassoside
  • Purification method of madecassoside

Examples

Experimental program
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Effect test

Embodiment 1

[0087] Add 300mL of anhydrous methanol and 20.00g of madecassoside to a 500ml reaction bottle in sequence, stir and mix for 10-15 minutes, stir and heat up to 60°C, after the complete dissolution of madecassoside, put the crystal system at 50°C, P Concentrate until the system reaches 8V under the condition of ≤-0.08MPa, then stop the concentration. Add 0.20g madecassoside to the crystallization system, naturally cool down to 25°C, heat and crystallize for 0.5-1.0 hours, filter the reaction system, take a sample of the filter cake for HPLC detection, after the relevant content is greater than 90%, put the filter cake at 55 Vacuum drying at -60°C and P≤-0.08MPa for 8-10 hours to obtain 16.2 g of refined madecassoside with a purity of 91.58%.

Embodiment 2

[0089] Add 360mL of anhydrous methanol and 20.00g of madecassoside to a 500ml reaction bottle in sequence, stir and mix for 10-15 minutes, stir and heat up to 65°C, after the complete dissolution of madecassoside, put the crystal system at 50°C, P Concentrate until the system reaches 7V under the condition of ≤-0.08MPa, then stop the concentration. Add 0.20g madecassoside to the crystallization system, naturally cool down to 25°C, heat and crystallize for 0.5-1.0 hours, filter the reaction system, and dry the filter cake in vacuum at 55-60°C, P≤-0.08MPa for 8- After 10 hours, 17.0 g of refined madecassoside was obtained with a purity of 91.00%.

Embodiment 3

[0091] Add 200mL of anhydrous methanol and 20.00g of madecassoside to a 500ml reaction bottle in turn, stir and mix for 10-15 minutes, stir and heat up to 60°C, after the complete dissolution of madecassoside, put the crystal system at 45°C, P Concentrate until the system reaches 8V under the condition of ≤-0.08MPa, then stop the concentration. Add 0.20g madecassoside to the crystallization system, naturally cool down to 20°C, heat and crystallize for 0.5-1.0 hours, filter the reaction system, and dry the filter cake in vacuum at 55-60°C, P≤-0.08MPa for 8- After 10 hours, 16.1 g of refined madecassoside was obtained with a purity of 90.42%.

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Abstract

The invention belongs to the field of medicines, and particularly relates to a purification method of madecassoside. The method specifically comprises the following steps of: (1) dissolving crude madecassoside by taking methanol as a solvent; (2) concentrating and evaporating to remove the solvent; (3) adding a seed crystal, cooling and crystallizing; and (4) filtering and drying. By selecting key influence factors such as the pulping solvent, the pulping solvent volume, the purification mode, the dissolution volume, the concentration and crystallization volume, the crystallization temperature, the drying mode and temperature, and the like, the madecassoside crystal nucleation and crystal growth speed are effectively controlled, so that the crystal quality of the product is ensured. By using the purification method provided by the invention, white or off-white crystalline powder can be obtained, the residual methanol solvent is less than 0.3%, and the content of madecassoside is higher than 90%.

Description

technical field [0001] The invention belongs to the field of medicine, and in particular relates to a purification method of madecassoside. Background technique [0002] Madecassoside, also known as madecassoside, English name Madecassoside, its CAS number is 34540-22-2, molecular formula: C 48 h 78 o 20 , molecular weight: 975.13, structure as shown in formula Ⅰ: [0003] [0004] Modern pharmacological studies have reported that madecassoside has the functions of removing scars and promoting wound healing, and can be used to treat skin ulcers, such as intractable wounds, skin tuberculosis, and leprosy. At present, total glycosides of Centella asiatica are mainly extracted from Centella asiatica, which contains triterpenoids, polyynyl olefins, flavonoids, alkaloids and polyphenols (including n-hexacane, 2,4, 6-tri-tert-butylbenzene, β-sitosterol, lauric acid, kaempferol, p-hydroxybenzoic acid, stigmasterol-3-O-β-D-glucose, asiatic acid, hydroxyasiatic acid, terminal ...

Claims

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Application Information

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IPC IPC(8): C07J63/00
CPCC07J63/008
Inventor 张亮扈靖胡杰
Owner INCREASEPHARM TIANJIN INST CO LTD
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