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Method for preparing high-purity prissine by high-speed countercurrent chromatography

A technology of high-speed countercurrent chromatography and prissine, applied in the field of high-speed countercurrent chromatography to prepare high-purity prissine, to achieve the effects of reducing changes in chemical properties, short separation time, and mild conditions

Inactive Publication Date: 2011-12-07
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

[0017] 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.

[0018] 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 pumped into the mobile phase (lower phase) and the stationary phase (upper phase)...

Embodiment 2

[0020] 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 to 254nm, and the peak of priscarin appears about 295 minutes after the sample in...

Embodiment 3

[0022]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, set the wavelength to 254nm, and the peak of priscarin appears about 105 minutes af...

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PUM

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Abstract

The invention discloses a method for preparing high-purity glenoid by high-speed countercurrent chromatography, which comprises the following steps: preparing a solvent system constituting a stationary phase and a mobile phase; adjusting the flow rate of the mobile phase; It is composed of petroleum ether, ethanol and water, the volume ratio of the three components is 9-12:9-10:1-1.1, the upper phase of the solvent system is a stationary phase, and the lower phase is a mobile phase. The method has mild separation conditions, high separation efficiency, and short separation time, and can obtain high-purity glenoidin.

Description

technical field [0001] The invention relates to a method for preparing high-purity prissine 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 Medical 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. Pristmerin is a pentacyclic triterpenoid compound with strong pharmacological activity, which has significant anti-tumor and anti-inflammatory activities. [0003]...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00C07J75/00B01D15/30
Inventor 杨培明肖婕妤欧阳丹薇倪翔许海燕陈佳
Owner SHANGHAI INST OF PHARMA IND CO LTD
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