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Preparation method of terpenoid

A technology of terpenoids and crude extracts, which is applied in the field of preparation of terpenoids, can solve the problems of large consumption of reagents, long time, and long time period, and achieve good operability, high repeatability, and abundant resources. Effect

Inactive Publication Date: 2015-03-25
TIANJIN YAOYU BIOLOGICAL TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] However, regarding the chemical composition of Kansui, the traditional extraction method is carried out by liquid-liquid extraction, which has the following defects: (1) There is no repeatability between batches, that is, the substance obtained by the first batch of extraction cannot be guaranteed The consistency between the components and the material components obtained by the second batch of extraction; (2) the distribution process of the material in different solvents takes a very long time, and it needs to be extracted multiple times (generally three times, each time a new solvent is replaced) ), and then combined, which results in a long time period for the entire extraction process and a large amount of reagent consumption

Method used

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  • Preparation method of terpenoid
  • Preparation method of terpenoid
  • Preparation method of terpenoid

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Use kansui as raw material, grind it into powder, heat it with ethyl acetate in a water bath at 60°C for 5 hours, extract it three times continuously, take the supernatant and concentrate it by distillation under reduced pressure to obtain the crude extract of ethyl acetate in the form of extract shape. Take by weighing 30g, be dissolved in 400mL ethanol volume fraction and be 40% ethanol-n-hexane solution, make Radix Gansui extract solution, concentration is 75mg / mL, cross 0.45 μ m microporous membrane, carry out one-dimensional liquid chromatography preparation, The chromatographic column is Innoval silica (250mm×150mm; 10μm, ), the mobile phase is a binary mixed organic phase, wherein phase A is n-hexane, phase B is ethanol, gradient elution mode: 0-37.5% B elution 30min, 100% B elution 10min. Using a UV detector, the detection wavelength is 210nm, the preparation temperature is room temperature, the injection volume is 200mL / needle, the flow rate of the mobile pha...

Embodiment 2

[0031]Use kansui as raw material, grind it into powder, heat it with ethyl acetate in a water bath at 60°C for 5 hours, extract it three times continuously, take the supernatant and concentrate it by distillation under reduced pressure to obtain the crude extract of ethyl acetate in the form of extract shape. Take by weighing 35g, be dissolved in 500mL ethanol volume fraction and be 50% ethanol-n-hexane solution, make the Radix Gansu extract solution, concentration is 70mg / mL, cross 0.45 μ m microporous membrane, carry out one-dimensional liquid chromatography preparation, The chromatographic column is Innoval silica (250mm×150mm; 10μm, ), the mobile phase adopts a binary mixed organic phase, wherein phase A is n-hexane, phase B is ethanol, and the gradient elution method: 0-37.5% phase B is eluted for 30 minutes, and 100% B is eluted for 10 minutes. Using a UV detector, the detection wavelength is 210nm, the preparation temperature is room temperature, the injection volume ...

Embodiment 3

[0033] Use kansui as raw material, grind it into powder, heat it with ethyl acetate in a water bath at 60°C for 5 hours, extract it three times continuously, take the supernatant and concentrate it by distillation under reduced pressure to obtain the crude extract of ethyl acetate in the form of extract shape. Weigh 45.5g, dissolve it in 700mL of ethanol-n-hexane solution with ethanol volume fraction of 60%, and obtain a solution of Gansui extract with a concentration of 65mg / mL, pass through a 0.45 μm microporous membrane, and carry out one-dimensional liquid chromatography preparation , the chromatographic column is Innoval silica (250mm×150mm; 10μm, ), the mobile phase adopts a binary mixed organic phase, wherein phase A is n-hexane, phase B is ethanol, and the gradient elution method: 0-37.5% phase B is eluted for 30 minutes, and 100% B is eluted for 10 minutes. Using a UV detector, the detection wavelength is 210nm, the preparation temperature is room temperature, the i...

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Abstract

The invention relates to a preparation method of a terpenoid. The method comprises steps as follows: a three-dimensional liquid chromatography technology is adopted, hexane-ethanol is taken as a mobile phase, a normal-phase silica-gel chromatographic column is taken as a one-dimensional preparation chromatographic column, component cutting is performed on an Euphorbia kansui extract, and a target component is collected as a one-dimensional separation component; then X-Amide (250 mm*20 mm) is taken as a two-dimensional preparation chromatographic column, component cutting, collection as well as rotating evaporation and concentration are performed on the one-dimensional separation component, a two-dimensional separation component is obtained, then X-Amide (250 mm*10 mm) is taken as a two-dimensional preparation chromatographic column, high-purity kansuinin B is obtained, and the highest purity can be higher than 98%; the whole preparation process is high in repeatability and good in operability, meanwhile, Euphorbia kansui resources are abundant, easy to obtain and suitable for large-scale production.

Description

technical field [0001] The invention relates to the field of compound production, in particular to a preparation method of terpenoids. Background technique [0002] Terpenoids (Terpenoids) are a class of important natural medicinal chemical components with diverse skeletons, large quantities, and extensive biological activities. The main components of the traditional Chinese medicine Gansui are such compounds, including triterpenoids and diterpenoids, and the pseudobaelone-type diterpenoids are one of the diterpenoids of Gansui, mostly a 5-membered ring and a 12-membered ring. The rings are formed by joining together, and the hydroxyl groups at certain positions form ether or ester bridges. Kansuinin B (kansuinin B) is one of them, which has a wide range of biological activities, and its structure is as follows: [0003] [0004] At present, it is found that kansuinin B has the activity of inhibiting cell division, and has certain biological activity in anti-tumor effec...

Claims

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Application Information

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IPC IPC(8): C07D303/32C07D301/32
CPCC07D301/32C07D303/32C07D307/00C07D493/08
Inventor 张耀洲马红
Owner TIANJIN YAOYU BIOLOGICAL TECH
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