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Method for separating rubescensinA from rabdosia

A technology of Rubescensin A and Rubescensin, which is applied in the field of separating and preparing monomer Rubescensin A from the crude product of Rubescensus A by countercurrent chromatography, and can solve the problem of unstable chemical properties of Rubescensin A, which is very difficult to solve. Difficult to obtain compound monomers, difficult separation work, etc., to achieve the effect of peak resolution, large separation amount, and solvent saving

Inactive Publication Date: 2006-04-26
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the chemical properties of oridonin are extremely unstable, which brings certain difficulties to the separation work
Moreover, when traditional separation techniques such as thin-layer chromatography and column chromatography are used, tailing, pollution, and loss are often caused by the adsorption of solid carriers, and it is difficult to obtain relatively high-purity compound monomers

Method used

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  • Method for separating rubescensinA from rabdosia
  • Method for separating rubescensinA from rabdosia
  • Method for separating rubescensinA from rabdosia

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 1. Heat and reflux 5kg of dried Radix Herba radix with 10L of 95% ethanol for 3 times, each time for 2 hours, filter out the solvent, add 10L of 95% ethanol to the filter residue, repeat the above operation three times, and dissolve the extract Combined and concentrated under reduced pressure with a vacuum rotary evaporator to form an extract, the concentration temperature is 40°C, and after drying, 200g of Oridinus crude product is obtained. The resulting crude product is subjected to normal phase silica gel column chromatography, the column size is: 150cm × 8cm, and the volume ratio of petroleum ether and acetone is 8:1, 6:1, 4:1, 2:1, 1:1. Elution, the flow rate is 10-15ml / min, obtains the crude product of oridonin, and its HPLC analysis is as follows: figure 1 As shown, the content of oridonin was 65.8%.

[0021] 2. Separation of Rubescensin A extract by countercurrent chromatography. Use n-hexane, ethyl acetate, methanol and water to prepare a two-phase solvent i...

Embodiment 2

[0023] The crude product of oridonin was prepared in the same manner as in Example 1, and the extract of oridonin was separated by countercurrent chromatography. Use petroleum ether, ethyl acetate, ethanol and water to prepare a two-phase solvent in a volume ratio of 1.5:2.5:1.5:2.5, put it in a liquid separation container to separate layers, and separate the upper and lower phases. Dissolve 300 mg of crude oridonin A in 8 ml of the upper phase and 8 ml of the lower phase to form a sample solution. The internal diameter of the countercurrent chromatographic column is 2.6mm, and the column volume is 850ml. The above phase is used as the stationary phase, and the lower phase is the mobile phase. After the separation column of the countercurrent chromatograph is filled with the stationary phase, the sample solution is injected into the sampling loop of the countercurrent chromatograph, and the countercurrent chromatograph is turned on at a speed of 500 rpm. The flow rate of 3ml / ...

Embodiment 3

[0025] The crude product of oridonin was prepared in the same manner as in Example 1, and the extract of oridonin was separated by countercurrent chromatography. Use chloroform, methanol and water to prepare a two-phase solvent in a volume ratio of 4:3:2, put it in a liquid separation container and separate the layers to separate the upper and lower phases. Dissolve 150 mg of crude oridonin A in 5 ml of the upper phase and 5 ml of the lower phase to form a sample solution. The internal diameter of the countercurrent chromatographic column is 1.6mm, and the column volume is 320ml. The above phase is used as the stationary phase, and the lower phase is the mobile phase. After the separation column of the countercurrent chromatograph is filled with the stationary phase, the sample solution is injected into the sampling loop of the countercurrent chromatograph, and the countercurrent chromatograph is turned on at a speed of 800 rpm. The flow rate of 1.5ml / min was injected into th...

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Abstract

The method of separating oridonin from rabdosia is one continuous liquid-liquid distributing adverse current chromatographic method without needing of any solid support and thus caused adsorption, loss, property change and other troubles. The method has high peak form resolution, great separation amount, no sample loss, high recovering rate, mild separating circumstance and low solvent consumption, and may be used in separating great amount of coarse oridonin product to reach purity over 97 %. In addition, the present invention adopts relatively simple and cheap adverse current chromatograph and economic mixture solvent comprising two or more of normal alkane, halohydrocarbon, fatty alcohol, aliphatic ketone, aliphatic ester, ether and water.

Description

technical field [0001] The invention relates to a method for isolating oridonin from Rubescens sativa, in particular to a method for separating and preparing monomer oridonin from a crude product of Rubescens sativa by countercurrent chromatography. Background technique [0002] Rubescensin A is one of the main diterpene components in Rubescens japonicus, and its structural formula is shown in formula I: [0003] [0004] Formula I [0005] Rabdosia rubescens, whose scientific name is Rabdosia rubescens Hera., is a plant belonging to the family Lamiaceae, which is produced in Shanxi, Henan and Hebei in my country. Chinese scientists discovered in the 1970s that its main component, Rubescensin A, has significant anticancer activity. Studies in recent years have also shown that Rubescensin A has good anti-tumor effects and has no obvious toxicity. Therefore, the research work on Rubescensin A has received extensive attention from scientists....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/02
Inventor 潘远江卢延斌
Owner ZHEJIANG UNIV
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