Method for extracting oridonin from rabdosia rubescens and purifying oridonin

A technology of Rubescensin A and a purification method, which is applied in the field of extracting and purifying Rubescensin A, can solve the problems of poor water-soluble effect, low yield, and poor effect of resin adsorption and enrichment of Rubescensin A, and achieve the goal of removing Good miscellaneous effect, good selectivity, and the effect of reducing dissolution

Inactive Publication Date: 2010-09-01
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent 03151477.4 (Application No.) "A Process for Extracting Rubescensine A from Rubescens japonicus" discloses methods such as extraction with ethanol, concentrated water redissolution, macroporous resin adsorption, silica gel magnesium oxide mixed column separation, recrystallization, etc. method, this method is suitable for industrialization, but the water-soluble effect of oridonin is poor, the resin adsorption and enrichment effect is poor, and the yield is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 20 kg of Rubescens grass raw material (0.7% oridonin content) and pulverize into 20 meshes, put it into a 500L extraction tank, add 160L of 70% methanol solution, add to 50°C, keep warm for dynamic extraction for 2 hours, suction filter the extract, add 120L of 70% methanol, kept at 50°C for dynamic extraction for 1 hour, suction filtered the solution, then added 120L of 70% 50°C for dynamic extraction at 50°C for 1 hour, suction filtered, combined three filtrates to obtain 360L, added 3.6 kg of activated carbon to reflux for decolorization for 1 hour, filtered, and reduced pressure Recover methanol to an alcohol concentration of 30%, release it, and cool to room temperature. Take 5 kg of ADS-17 resin for column packing and activation. Add the concentrated solution to the resin column for adsorption at a flow rate of 5L / h. After saturated adsorption (high performance liquid phase monitoring during the adsorption process), first elute impurities with 30L of water at...

Embodiment 2

[0031] Take 20 kg of Rubescens grass raw material (0.7% oridonin content) and pulverize into 40 meshes, put it into a 500L extraction tank, add 160L of 60% methanol solution, add to 60°C, keep warm for dynamic extraction for 2 hours, suction filter the extract, add 120L of 60% methanol, kept at 50°C for dynamic extraction for 1 hour, extracted twice and filtered the solution, combined three filtrates to obtain 360L, added 1.8 kg of activated carbon to reflux for decolorization for 0.5 hours, filtered, recovered methanol under reduced pressure until the alcohol concentration was 20%, released , to cool down to room temperature. Take 7 kg of ADS-7 resin for column packing and activation. Add the concentrated solution to the resin column for adsorption at a flow rate of 7L / h. After saturated adsorption (high performance liquid phase monitoring during the adsorption process), firstly use 35L of water to elute impurities at a flow rate of 15L / h, and then use 35L of 85% methanol to ...

Embodiment 3

[0033] Take 20 kg of Rubescensia raw material (0.7% oridonin content) and pulverize into 20 meshes, put it into a 500L extraction tank, add 160L of 70% methanol solution, add to 60°C, keep warm for dynamic extraction for 2 hours, filter the extract, add 160L of 70% methanol, kept at 60°C for dynamic extraction for 1 hour, suction filtered the solution, combined the filtrates to obtain 280L, added 1.6 kg of activated carbon to reflux for decolorization for 0.5 hours, filtered, recovered methanol under reduced pressure to an alcohol concentration of 30%, released, and cooled to room temperature. Take 5 kg of ADS-17 resin for column packing and activation. Add the concentrated solution to the resin column for adsorption at a flow rate of 2.5L / h. After saturated adsorption (high performance liquid phase monitoring during the adsorption process), first elute impurities with 30L of water at a flow rate of 15L / h, and then wash with 25L of 85% methanol at a flow rate of 3L / h. Deoridid...

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Abstract

The invention discloses a novel process for extracting oridonin from rabdosia rubescens and purifying the oridonin. In the process, extraction is performed in 60 to 70 percent ethanol for 2 to 3 times, active carbon is used for decolorization, the extract is condensed under reduced pressure till the concentration of the methanol is 20 to 30 percent, macroporous resin absorption is performed, 75 to 85 percent methanol is used for elution, condensation is performed, extraction is performed step by step by using petroleum ether and ethyl acetate, ethyl acetate extracting solution is recovered, a small amount of petroleum ether is added, the solution is stood for crystallization, and refluxing and saturated dissolution and crystallization in 70 percent methanol and 90 percent methanol are performed in turn. The process is simple and is easy in operation.

Description

Technical field: [0001] The invention relates to a method for extracting and purifying oridonin from Rubescens sativa. The method is a method for purifying oridonin by adopting low-alcohol state resin adsorption, extraction and crystallization. Background technique: [0002] Oridonin is also called Oridonin and Yanming Caoning. [0003] Molecular formula: C20H28O6 [0004] Molecular weight: 364.43 [0005] Physical properties: melting point 248°C-250°C, slightly soluble in water, soluble in methanol, ethyl acetate, acetone, etc. [0006] Oridonin A is a tetracyclic diterpenoid isolated from the traditional Chinese medicine Oridonin. The role of oridonin in cancer treatment has attracted people's attention, and it has been found that it has inhibitory effects on various cell lines such as lung cancer, prostate cancer, and breast cancer. [0007] Donglingcao, also known as Binglingcao, Yanmingcao, Caihuacao, etc., is a perennial herb or subshrub of Lamiaceae Fragrant Tea. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/08
Inventor 刘东锋张翼杨成东
Owner NANJING ZELANG MEDICAL TECH
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