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Method for preparing lactuca indica and lactucin

A technology for the separation of radish and radish, which is applied in the field of preparation of the separation of radish and radish, and can solve problems such as poor repeatability, large instrument damage, and poor solubility

Active Publication Date: 2013-08-14
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It has been reported to separate radish and radish from chicory root by n-hexane-ethyl acetate-methanol-water (1.5:4:2.5:6) and ethyl acetate-methanol-water (20:2:20) systems. lettucein and other sesquiterpene components, but there are still some problems when using these solvent systems, firstly, the retention of the stationary phase is not good, and the repeatability is poor, and secondly, the ethyl acetate part of the root extract of Chicory is dissolved in these solvent systems Poor solubility, resulting in less sample loading and greater damage to the instrument, so it is very important to find a solvent system or solvent that improves solubility or helps solubility

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Take 500 g of chicory root and pulverize it, then use 70% ethanol to extract it by ultrasonic extraction, the liquid ratio is 1:5, the extraction temperature is 20°C, the extract is concentrated under reduced pressure until it has no alcohol smell, and the total extract is obtained;

[0019] Disperse the total extract in water, sequentially extract with petroleum ether, ethyl acetate, and n-butanol, and distill under reduced pressure to obtain the extracts of petroleum ether, ethyl acetate, and n-butanol respectively;

[0020] Take 1.5g of the extract from the part of ethyl acetate, dissolve it in ethyl acetate, separate it by 200-mesh silica gel column chromatography, and elute with the gradient of n-hexane-ethyl acetate solvent system at a volume ratio of 4-1:1-3. Collect 15-20ml, carry out follow-up inspection on the fractions by thin-layer chromatography (TLC), use petroleum ether: ethyl acetate 1:5 as the developing solvent, combine the same components, concentrate ...

Embodiment 2

[0025] After taking 500 g of chicory root and pulverizing it, use 90% ethanol to extract with the help of ultrasound, the liquid ratio: 1:10, the extraction temperature is 30 ° C, the extract is concentrated under reduced pressure until it has no alcohol smell, and the total extract is obtained;

[0026] Disperse the total extract in water, sequentially extract with petroleum ether, ethyl acetate, and n-butanol, and distill under reduced pressure to obtain the extracts of petroleum ether, ethyl acetate, and n-butanol respectively;

[0027] Take 1.5g of the extract from the part of ethyl acetate, dissolve it in ethyl acetate, separate it by 300-mesh silica gel column chromatography, and elute with the gradient of n-hexane-ethyl acetate solvent system at a volume ratio of 4-1:1-3. Collect 18ml, carry out follow-up inspection of the fractions by thin-layer chromatography (TLC), use petroleum ether: ethyl acetate 1:5 as the developing solvent, combine the same components, concentra...

Embodiment 3

[0032] After taking 500 g of chicory root and pulverizing it, extract it with anhydrous methanol by hot reflux extraction, the liquid ratio is 1:15, the temperature is 60°C, the extract is concentrated under reduced pressure until it has no alcohol smell, and the total extract is obtained;

[0033] Disperse the total extract in water, sequentially extract with petroleum ether, ethyl acetate, and n-butanol, and distill under reduced pressure to obtain the extracts of petroleum ether, ethyl acetate, and n-butanol respectively;

[0034] Take about 1.5 g of the extract from the part of ethyl acetate, dissolve it in ethyl acetate, separate it by 200-mesh silica gel column chromatography, and elute with a gradient of n-hexane-ethyl acetate solvent system at a volume ratio of 4-1:1-3. Parts collected 20ml, and the fractions were tracked and checked by thin-layer chromatography (TLC), using sherwood oil: ethyl acetate 1: 5 as a developing solvent, combining the same components, and conce...

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PUM

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Abstract

The invention relates to a method for preparing lactuca indica and lactucin, which is a method for using two separation processes to obtain lactuca indica and lactucin from cichorium glandulosum by a high-speed countercurrent chromatography. The method has the advantages of large fractional dose, small sample loss, high recovery rate, mild separation environment and solvent saving. A great amountof lactuca indica and lactucin crude products can be placed in a countercurrent chromatograph, the separation result achieves the high purity and good separation effect. The method is not only suitable for preparing the product with high purity from plant crude extract, but also suitable for purifying lactuca indica and lactucin crude extracts obtained by various approaches.

Description

technical field [0001] The invention relates to a preparation method for separating beletin and beletin from chicory by using high-speed countercurrent chromatography. Background technique [0002] Chicory is an annual herbaceous plant belonging to the genus Chicory of the Compositae family. It is a commonly used medicinal material of the Uyghur nationality. Its aerial part is used as medicine. Recently, it was found that the extract of chicory root has the effects of protecting the liver, lowering blood sugar, and lowering blood fat, and the seed extract has the effect of anti-hepatotoxicity. [0003] In recent decades, domestic and foreign scholars have continuously deepened the research on the phytochemistry of Cichorium. The research of domestic and foreign scholars mainly focuses on Cichorium (Cichoriumi intybus L.). Chemical research shows that: its main components include various terpenoids, flavonoids Cichorium glandulosum Boiss.et Huet. As a plant of the same genus...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/93
Inventor 信学雷张尧阿吉艾克拜尔·艾萨杨义巴杭
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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