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
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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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