A method for separating and purifying alderone, pinenin, cardamonin and alpinol from cardamom

A technology of separation and purification and cardamonin, which is applied in the separation/purification of carbonyl compounds, organic chemistry, bulk chemical production, etc., can solve the problems of difficult expansion of separation scale, residual organic reagents, and large consumption of organic solvents, etc., to achieve easy Automatic control, easy recycling and low production cost

Active Publication Date: 2018-03-09
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the purity of the compound obtained by column chromatography is high, the operation is cumbersome, the choice of solvent system in high-speed countercurrent chromatography is difficult, and the separation scale is difficult to expand
In addition, both methods need to consume a large amount of organic solvents. The recovery cost of organic solvents is high, recycling is difficult, and the residue of organic reagents in the product is serious, which is harmful to the environment and human health.

Method used

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  • A method for separating and purifying alderone, pinenin, cardamonin and alpinol from cardamom
  • A method for separating and purifying alderone, pinenin, cardamonin and alpinol from cardamom

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 100 g of cardamom, pulverize it with a grinder, put it into a glass container, add 1000 ml of 70% ethanol, ultrasonically extract 3 times, each time for 0.5 hours, combine the extracts, filter, and concentrate under reduced pressure to obtain cardamom extract.

[0025] The cardamom extract is dissolved in methanol, filtered, and separated by supercritical fluid chromatography. The chromatographic column is a diol-based column, and the temperature of the chromatographic column is 35°C. The mobile phase was supercritical carbon dioxide, the flow rate was 3 times column volume / min, and the pressure was 11 MPa. Modifier is ethanol, its proportion is 10%. The separation process was detected by an ultraviolet detector with a detection wavelength of 300nm. The fractions of the target components were collected according to the detection signals, and four compounds of alderone, pinenin, cardamonin and alpinol were obtained respectively.

Embodiment 2

[0027] Weigh 100 g of cardamom, crush it with a grinder, put it into a glass container, add 1500 ml of 70% ethanol, ultrasonically extract 3 times, each time for 0.5 hours, combine the extracts, filter, and concentrate under reduced pressure to obtain cardamom extract.

[0028] The cardamom extract is dissolved in methanol, filtered, and separated by supercritical fluid chromatography. The chromatographic column is a diol-based column, and the temperature of the chromatographic column is 30°C. The mobile phase was supercritical carbon dioxide, the flow rate was 4 times column volume / min, and the pressure was 10 MPa. Modifier is ethanol, its proportion is 8%. The separation process was detected by an ultraviolet detector with a detection wavelength of 300 nm. The fractions of the target components were collected according to the detection signals, and four compounds of alderone, pinenin, cardamonin and alpinol were obtained respectively.

Embodiment 3

[0030] Weigh 100 g of cardamom, pulverize it with a grinder, put it into a glass container, add 500ml of 70% ethanol, ultrasonically extract 3 times, each time for 1.5 hours, combine the extracts, filter, and concentrate under reduced pressure to obtain cardamom extract.

[0031] The cardamom extract is dissolved in methanol, filtered, and separated by supercritical fluid chromatography. The chromatographic column is a diol-based column, and the temperature of the chromatographic column is 40°C. The mobile phase is supercritical carbon dioxide, the flow rate is 2.5 times column volume / min, and the pressure is 12 MPa. Modifier is ethanol, its proportion is 7%. The separation process was detected by an ultraviolet detector with a detection wavelength of 300 nm. The fractions of the target components were collected according to the detection signals, and four compounds of alderone, pinenin, cardamonin and alpinol were obtained respectively.

[0032] Through HPLC area normalizati...

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Abstract

The invention provides a method for separating and purifying alnustone, pinocembrin, cardamomin and alpinetin from alpinia katsumadai. Alpinia katsumadai is smashed, 70% ethanol is added for ultrasonic extraction, an extraction solution is filtered and subjected to vacuum concentration to obtain an alpinia katsumadai extract; the extract is dissolved with methanol, supercritical fluid chromatographic separation is conducted after filtering, a chromatographic column is a diol column, a mobile phase is supercritical CO2 fluid, and ethanol serves as a modifier. Carbon dioxide serves as a main mobile phase, a small quantity of organic solvent is added to serve as the modifier, harm to the environment and body health is small, recycling of carbon dioxide is easy, energy consumption is low, production cost is low, the production process is environmentally friendly, products are easy to recycle, and the obtained products are free of harmful matter and residues.

Description

technical field [0001] The invention belongs to the fields of chemical industry and pharmacy, and in particular relates to a supercritical fluid chromatography method for separating and purifying alderone, pinenin, cardamonin and alpinol from cardamom extract. Background technique [0002] Cardamom grass is the dry and nearly mature seed mass of cardamom grass, a plant in the ginger family. It is fragrant, pungent, and slightly bitter. It has the functions of drying dampness and invigorating the spleen, warming the stomach and relieving vomiting. Full of cold pain, belching and vomiting, not thinking about eating and other symptoms. Preliminary studies have shown that alpinol, joconin, cardamonin, and alderone have the highest content in cardamom, and have pharmacological effects such as anti-inflammatory, antibacterial, hypoglycemic, anti-oxidation, anti-radiation, anti-cancer, anti-tumor, and enhancing immunity . [0003] The separation methods of the effective component...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/32C07D311/40C07C45/78C07C45/79C07C45/80C07C49/223C07C49/84
CPCC07C45/78C07C45/79C07C45/80C07D311/32C07D311/40C07C49/223C07C49/84Y02P20/54
Inventor 王延翠孙爱玲李爱峰秦秀秀柳仁民
Owner LIAOCHENG UNIV
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