Method for preparing high-purity demethylzelasteral

A xylaldehyde, mobile phase technology, applied in the direction of pharmaceutical formulations, medical preparations containing active ingredients, steroids, etc., to achieve the effects of mild conditions, broad application prospects, and short separation time

Inactive Publication Date: 2012-05-23
SHANGHAI INST OF PHARMA IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no complete set of theoretical basis for the selection of solvent system.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] High-speed counter-current chromatography to obtain zera wood aldehyde:

[0025] 100 grams of dried root bark of Snakevine (produced in the southern mountainous area of ​​Hunan Province) was extracted by cold immersion in dichloromethane, each cold immersion was 24 hours, and then the solvent was recovered, and repeated three times to obtain a brown dry powdery substance, which is called crude extraction and drying. thing, accurately weighed 11.2 grams of dichloromethane rough extraction dry matter.

[0026] Accurately weigh 1 gram of dichloromethane rough extraction dry matter, dissolve the sample with the upper phase of the solvent system of petroleum ether: ethanol: water (solvent volume ratio 10: 10: 1), open the constant temperature circulator, set the temperature to 25 degrees Celsius, and The upper phase of the solvent system is the stationary phase, and the lower phase is the mobile phase. The mobile phase (lower phase) and the stationary phase (upper phase) are...

Embodiment 2

[0028] High-speed counter-current chromatography to obtain zera wood aldehyde:

[0029]Accurately weigh 1.2 grams of dichloromethane crude extraction dry matter, use petroleum ether: ethanol: water (solvent volume ratio 10: 9: 1) upper phase dissolving sample of solvent system, open constant temperature circulator, setting temperature is 24 degrees Celsius, with The upper phase of the solvent system is the stationary phase, and the lower phase is the mobile phase. The mobile phase (lower phase) and the stationary phase (upper phase) are pumped into the mobile phase (lower phase) and the stationary phase (upper phase) at the same time with double pumps. Phase, set the flow rate of the mobile phase to 1.8ml / min, turn on the host motor at the same time, adjust the speed to 860rpm, after ten minutes, the solvent system in the column reaches a dynamic equilibrium, and only the mobile phase flows out from the column outlet. Inject the sample through the injector, set the wavelength ...

Embodiment 3

[0031] High-speed counter-current chromatography to obtain zera wood aldehyde:

[0032] Accurately weigh 1.6 grams of dichloromethane crudely extracted dry matter, dissolve the sample in the upper phase of the solvent system with petroleum ether: ethanol: water (solvent volume ratio 9: 10: 1), open the constant temperature circulator, set the temperature to 23 degrees Celsius, and The upper phase of the solvent system is the stationary phase, and the lower phase is the mobile phase. The mobile phase (lower phase) and the stationary phase (upper phase) are pumped into the mobile phase (lower phase) and the stationary phase (upper phase) at the same time with double pumps. Phase, set the flow rate of the mobile phase to 2.2ml / min, turn on the host motor at the same time, adjust the speed to 840rpm, after ten minutes, the solvent system in the column reaches a dynamic equilibrium, and only the mobile phase flows out from the column outlet. Inject the sample through the injector, ...

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PUM

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Abstract

The invention discloses a method for preparing high-purity demethylzelasteral, which is characterized in that the demethylzelasteral is obtained by being separated from a plant called oriental biter wThe invention discloses a method for preparing high-purity demethylzelasteral, which is characterized in that the demethylzelasteral is obtained by being separated from a plant called oriental biter weed, and high-speed countercurrent chromatography is preferably adopted. The method has the advantages of gentle separating condition, high separating efficiency and short separating time and can obtaeed, and high-speed countercurrent chromatography is preferably adopted. The method has the advantages of gentle separating condition, high separating efficiency and short separating time and can obtain high-purity demethylzelasteral.in high-purity demethylzelasteral.

Description

technical field [0001] The invention relates to a method for isolating and obtaining high-purity zeramualdehyde from S. chinensis plants, in particular to a method for separating and obtaining high-purity zeramualdehyde from S. henifolia plants by high-speed countercurrent chromatography (HSCCC). Background technique [0002] Celastrus orbiculatus Thumb is a commonly used plant medicine in my country. It has the effects of dispelling wind and dehumidification, promoting blood circulation, detoxifying and reducing swelling. , Sha syndrome, dysentery, swollen poison, bruises (Shou Liren. Modern Dictionary of Chinese Materia Medica (Volume 2) [M]. Beijing: People's Health Publishing House. 2001.1457). The main medicinal components of S. serpentine are sesquiterpenes and sesquiterpene derivatives, alkaloids, triterpenes, and flavonoids. Among them, triterpenoids mainly exist in the root bark of S. genus. The main types There are lupine type and oleanolic acid type. Zeylasteral...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00A61K31/56A61K36/37A61P31/00
Inventor 肖婕妤杨培明欧阳丹薇倪翔许海燕陈佳
Owner SHANGHAI INST OF PHARMA IND CO LTD
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