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A method for rapidly preparing emodin and emodin

A technology of emodin and emodin, applied in chemical instruments and methods, ether preparation, sugar derivative preparation and other directions, to achieve the effects of reducing organic solvent consumption and energy consumption, stable properties, and solvent saving

Active Publication Date: 2016-05-25
CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, it takes at least 320 minutes for these patents to completely separate the two compounds during the separation process.
Therefore, the high-speed countercurrent chromatography preparation method using chloroform-n-butanol-methanol-water as a two-phase solvent system has certain limitations in the actual production and application in the pharmaceutical and health food industries

Method used

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  • A method for rapidly preparing emodin and emodin
  • A method for rapidly preparing emodin and emodin
  • A method for rapidly preparing emodin and emodin

Examples

Experimental program
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Effect test

Embodiment 1

[0058] A method for rapidly separating and preparing emodin and emodin from fenugreek by high-speed countercurrent chromatography, comprising the following steps:

[0059] (1) The fenugreek seeds crushed to 40 meshes are 1g to 10ml, and the ethanol aqueous solution with a mass percentage concentration of 40% is added to extract under reflux for 3 times, and the extracts are combined and concentrated to dryness at 60°C to obtain a solid The substance mass percentage content is 35% fenugreek extract.

[0060] (2) Dissolve the fenugreek extract with deionized water at 1g:5mL, extract twice with an equal volume of petroleum ether, combine the lower supernatants and extract twice with an equal volume of ethyl acetate, and combine the lower supernatants Then extract twice with an equal volume of n-butanol, combine the upper layer extracts, concentrate, and concentrate under reduced pressure at 50°C to obtain a sample to be separated with a solid content of 15% by mass; the high-effi...

Embodiment 2

[0070] A method for rapidly separating and preparing emodin and emodin from fenugreek by high-speed countercurrent chromatography, comprising the following steps:

[0071] (1) The fenugreek seeds crushed to 60 mesh are 1g to 30ml, and the ethanol aqueous solution with a mass percentage concentration of 80% is added to extract under reflux for 3 times, and the extracts are combined and concentrated to dryness at 60°C to obtain a solid The mass percentage of the product is 62% fenugreek extract.

[0072] (2) Dissolve the fenugreek extract with deionized water at 1g:15mL, extract 10 times with an equal volume of petroleum ether, combine the lower supernatants with an equal volume of ethyl acetate for 10 times, combine the lower supernatants and then Extract with an equal volume of n-butanol for 10 times, combine the upper layer extracts, and concentrate under reduced pressure at 70°C to obtain a sample to be separated with a solid content of 30% by mass;

[0073](3) Mix the two-...

Embodiment 3

[0078] A method for rapidly separating and preparing emodin and emodin from fenugreek by high-speed countercurrent chromatography, comprising the following steps:

[0079] (1) Fenugreek seeds crushed to 50 meshes were added into 60% ethanol aqueous solution by mass percent at a ratio of 1:20 g / ml to extract by heating and refluxing for 3 times. The extracts were combined and concentrated to dryness at 60°C. The mass percent composition that obtains solid is the fenugreek extract of 57%.

[0080] (2) After dissolving the fenugreek extract with deionized water at 1g:10mL, extract 5 times with an equal volume of petroleum ether, combine the lower supernatants and extract 5 times with an equal volume of ethyl acetate, and combine the lower supernatants Then extract 5 times with an equal volume of n-butanol, combine the upper layer extracts, and concentrate under reduced pressure at 60°C to obtain a sample to be separated with a solid content of 27% by mass;

[0081] (3) Mix the t...

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Abstract

The invention discloses a method for quick separation and preparation of rhaponticin and rhapontigenin. The method comprises the following steps: 1) seeds of trigonella foenum-graecum L. Are crushed and then placed in ethanol water to be subjected to reflux extraction, and extract is collected and concentrated to obtain trigonella foenum-graecum L. extractive; 2) the trigonella foenum-graecum L. extractive is dissolved in deionized water and then extracted with ligarine, clear liquid on the lower layer is extracted with vinegar naphtha, clear liquid on the lower layer is extracted with n-butanol, and an extract liquor on the upper layer is concentrated to obtain a sample to be separated; 3) the sample to be separated is separated by high-speed counter-current chromatography to obtain fractions containing rhaponticin and rhapontigenin in sequence; a stationary phase and a mobile phase are prepared from normal hexane, vinegar naphtha, methanol and water at the volume ratio of (1-3):(6-10):(2-6):(10-14); an upper sample solution is prepared by dissolving the sample to be separated into the mobile phase. The method is simple and quick, ensures large preparation quantity and high product purity and is suitable for industrial mass production.

Description

technical field [0001] The invention relates to a method for rapidly preparing emodin and emodin. Background technique [0002] Both rhizoside and emodin belong to polyhydroxystilbene compounds, which are mainly a kind of phytoalexin produced by plants under unfavorable conditions such as fungal infection and strong ultraviolet radiation. Studies have found that polyhydroxystilbene compounds such as emodin and emodin have antibacterial and anti-inflammatory effects, promoting blood circulation and removing blood stasis, regulating blood sugar and inhibiting tumors and other significant pharmacological effects. Polyhydroxystilbene compounds were first discovered in rhubarb, a plant of Polygonaceae, which is also the main source of medicinal active ingredients such as rhubarb. In recent years, with the in-depth research and development of the pharmacological value of polyhydroxystilbene compounds, the demand for plant resources has gradually increased, and the phenomenon of o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/203C07H1/08C07C41/36C07C43/253
Inventor 王洪伦何彦峰王小艳丁晨旭索有瑞
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST