Method for enriching and purifying eugenol in Chinese pink herb

A technology of eugenol and dianthus, which is applied in the preparation of enrichment and purification of eugenol in dianthus by high-speed countercurrent chromatography separation method, and in the field of eugenol purification, which can solve the problems of low extraction purity and low extraction rate, and achieve no loss of samples , high recovery, fast liquid-liquid partition chromatography separation effect

Active Publication Date: 2013-06-05
HEILONGJIANG DINGHENGSHENG PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the shortcomings of conventional techniques such as relatively low extraction rate and low extraction purity, and provide a preparation method for enriching and purifying eugenol in caryophyllum by high-speed countercurrent chromatography

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Preparation of eugenol with a purity higher than 90% using ethyl acetate-n-butanol-water and chloroform-methanol-isopropanol-water two-solvent system: using a semi-preparative high-speed countercurrent chromatograph equipped with an NS-1007 pump, 20ml Injection valve, polytetrafluoroethylene column, the volume of the column is 240ml, 8823A-UV ultraviolet detector Yokogawa 3057 portable recorder. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 800rpm, and pump the mobile phase into the column at a flow rate of 2.0ml / min. Detector UV spectra to receive target components. The preparation of eugenol is carried out in two steps: (1) Ethyl acetate-n-butanol-water with a volume ratio of 2:3:1 is miscible in a separatory funnel, shaken and then separated into layers. Get the upper layer solution (upper phase) as the stationary phase, and the lower layer solution (lower phase) as the mobile phase. Dissolve 100 mg of...

Embodiment 2

[0017] Preparation of eugenol with a purity higher than 90% using ethyl acetate-isobutanol-acetone-water and chloroform-methanol-water two-solvent system: using a semi-preparative high-speed countercurrent chromatograph equipped with a NS-1007 pump, 20ml sample injection Valve, Teflon column, column volume 240ml, 8823A-UV ultraviolet detector Yokogawa 3057 portable recorder. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 800rpm, and pump the mobile phase into the column at a flow rate of 2.0ml / min. Detector UV spectrum to receive target components. The preparation of carotene is carried out in two steps: (1) Ethyl acetate-isobutanol-acetone-water with a volume ratio of 5:40:60:1 is miscible in a separatory funnel, shaken up and then separated into layers. Get the upper layer solution (upper phase) as the stationary phase, and the lower layer solution (lower phase) as the mobile phase. Dissolve 200 mg of crude ext...

Embodiment 3

[0019] Preparation of eugenol with a purity higher than 90% using n-butanol-water and dichloromethane-isopropanol-chloroform-methanol-water two-solvent system: using a semi-preparative high-speed countercurrent chromatograph equipped with an NS-1007 pump, 20ml Injection valve, polytetrafluoroethylene column, the volume of the column is 240ml, 8823A-UV ultraviolet detector Yokogawa 3057 portable recorder. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 800rpm, and pump the mobile phase into the column at a flow rate of 2.0ml / min. Detector UV spectrum to receive target components. The preparation of carotene is carried out in two steps: (1) n-butanol-water with a volume ratio of 45:5 is miscible in a separatory funnel, shaken and then separated into layers. Get the upper layer solution (upper phase) as the stationary phase, and the lower layer solution (lower phase) as the mobile phase. Dissolve 150 mg of crude extr...

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Abstract

The invention belongs to the field of natural organic chemistry and relates to a method for purifying eugenol, in particular to a preparation method for enriching and purifying eugenol in Chinese pink herb by using a high-speed countercurrent chromatographic separation method. The method is characterized by comprising the steps of: processing leach liquor of natural plant Chinese pink herb by using the high-speed countercurrent chromatographic separation method and purifying twice to obtain the eugenol with the purity of 90%. The method is suitable for natural plants containing the eugenol, and the extract of the natural plants is used as a raw material for preparing high-purity eugenol. The method is suitable for preparing the eugenol by adopting various models of countercurrent chromatographic instruments in a separation manner, liquid-liquid distribution chromatographic separation can be continuously, efficiently and rapidly carried out by adopting the high-speed countercurrent chromatographic method to prepare the eugenol, and the characteristics of high separation capacity, no sample loss, high recovery yield, alleviated separation environment, solvent saving and the like canbe achieved.

Description

Technical field: [0001] The invention belongs to the field of natural organic chemistry and relates to a method for purifying eugenol, in particular to a preparation method for enriching and purifying eugenol in dianthus by using a high-speed countercurrent chromatographic separation method. Background technique: [0002] Dianthus: Chinese Dianthus, Chinese Marsh Bamboo, Dianthus, Shizhuhua, Shiyangjinghua, Luoyang Flower, Wang Yinghua, Luoyang Dianthus, Shichrysanthemum, Xiuzhu, Evergreen, Sunset Grass, Dimegrass, etc. It is a perennial herbaceous plant of the genus Caryophyllaceae, which can be used as medicine in whole plant or root. It has the effects of clearing away heat and diuresis, breaking blood and promoting menstruation. The whole herb contains saponins and volatile oils, mainly eugenol, phenylethyl alcohol, benzyl benzoate, benzyl salicylate, and methyl salicylate in the oil. [0003] Eugenol is a natural active substance that has a significant health care eff...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/23C07C41/36
Inventor 姚德坤姚德利刘德文闫峰黄运生姚航郑君
Owner HEILONGJIANG DINGHENGSHENG PHARM CO LTD
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