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Lanostane triterpenoid preparing method

A technology of lanosterane and triterpenoids, which is applied in the field of preparation of lanosterane triterpenoids, can solve the problems of long extraction process, large consumption of reagents, non-repeatable batches, etc., and achieve consistency High, high degree of automation of the instrument, and the effect of reducing the workload

Inactive Publication Date: 2015-12-09
TIANJIN YAOYU BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, regarding the chemical components of Kansui, the traditional extraction method is carried out by liquid-liquid extraction, which has many defects, such as non-repeatability between batches, long time period of the entire extraction process, and large consumption of reagents Wait

Method used

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  • Lanostane triterpenoid preparing method
  • Lanostane triterpenoid preparing method
  • Lanostane triterpenoid preparing method

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Take kansui as raw material, grind it into powder, soak it in ethyl acetate at room temperature for 5 hours, the solid-liquid ratio of kansui coarse powder to ethyl acetate is 1:8 in kg / L, stir intermittently, and extract continuously for 3 times , take the supernatant and concentrate it by distillation under reduced pressure. Choose a vacuum degree of 0.05Mpa and a temperature of 50°C to obtain a crude ethyl acetate extract in the form of an extract; weigh 350g and dissolve it in 3800mL of ethanol with a volume fraction of 30% ethanol -n-hexane solution, the obtained Kansui extract solution, the concentration is 92mg / mL, pass through a 0.45 μm microporous membrane, and carry out one-dimensional liquid chromatography preparation, the chromatographic column is Innovalsilica (250mm×150mm; 10 μm, ), the mobile phase is a binary mixed organic phase, wherein phase A is n-hexane, phase B is ethanol, gradient elution mode: 0-20% B elution 25min, 100% B elution 8min. Using a UV...

Embodiment 2

[0037] Take kansui as raw material, grind it into powder, soak it in ethyl acetate at room temperature for 5 hours, the solid-liquid ratio of kansui coarse powder to ethyl acetate is 1:10 in kg / L, stir intermittently, and extract continuously for 3 times , take the supernatant and concentrate it by distillation under reduced pressure, choose a vacuum degree of 0.05Mpa, and a temperature of 50°C to obtain a crude extract of ethyl acetate in the form of an extract; weigh 380g, dissolve it in 4000mL of ethanol with a volume fraction of 30% ethanol -n-hexane solution, the prepared Kansui extract solution, the concentration is 95mg / mL, passes through 0.45 μm microporous membrane, carries out one-dimensional liquid chromatography preparation, and chromatographic column is Innovalsilica (250mm×150mm; 10 μm, ), the mobile phase is a binary mixed organic phase, wherein phase A is n-hexane, phase B is ethanol, gradient elution mode: 0-20% B elution 25min, 100% B elution 8min. Using a U...

Embodiment 3

[0039] Take kansui as raw material, grind it into powder, soak it with ethyl acetate at room temperature for 5 hours, the solid-liquid ratio of kansui coarse powder to ethyl acetate is 1:9 in kg / L, stir intermittently, and extract continuously for 3 times , take the supernatant and concentrate it by distillation under reduced pressure, select a vacuum degree of 0.05Mpa, and a temperature of 50°C to obtain a crude ethyl acetate extract in the form of an extract; weigh 400g, dissolve it in 4500mL of ethanol with a volume fraction of 30% ethanol -n-hexane solution, the prepared Gansui extract solution, the concentration is 89mg / mL, passes through 0.45 μm microporous membrane, carries out one-dimensional liquid chromatography preparation, and chromatographic column is Innovalsilica (250mm×150mm; 10 μm, ), the mobile phase is a binary mixed organic phase, wherein phase A is n-hexane, phase B is ethanol, gradient elution mode: 0-20% B elution 25min, 100% B elution 8min. Using a UV ...

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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 lanostane triterpenoids. Background technique [0002] Terpenoids (TerpenoiAs) are a class of important natural medicinal chemical components with diverse skeletons, large quantities and wide biological activities. The main components of the traditional Chinese medicine Gansui are such compounds, mainly including triterpenoids and diterpenoids. And lanosterane triterpenoids (3β, 11β)-3,11-dihydroxylanosta-8,24-dien-7-one is one of the triterpenoid components of Gansui, and its structure is as follows: [0003] [0004] Gansui included in the current "Chinese Pharmacopoeia" is the dry tuber root of Euphorbiaceae Euphorbia plant Gansui. Cold in nature, bitter in taste; poisonous. Modern studies have shown that the chemical constituents of Kansui have anti-oxidation, anti-tumor, anti-fertility, anti-virus, purgatory and immunosuppressive effects. [...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
CPCC07D301/32C07D303/32C07D307/00C07D493/08
Inventor 张耀洲马红杜思邈盖其静杨珊珊陆洪庞莉王欢欢韩朝李上文
Owner TIANJIN YAOYU BIOLOGICAL TECH
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