Process for extracting proanthocyanidin from grape seed by super critical carbon dioxide

Abstract

The supercritical CO2 process of extracting proanthocyanidin from grape seed includes the following steps: adding anhydrous ethyl alcohol as entrainer and grape seed after being supercritical deoiled in certain ratio into extracting kettle for extraction at 35-55 deg.c and 30-50 MPa; soaking statically for 30-90 min; adding entrainer continuously in certain ratio and discharging dynamically; twice separating the extracted solvent to obtain proanthocyanidin containing solvent; and evaporating the solvent to obtain proanthocyanidin product. The process of the present invention has reduced entrainer consumption, short production period, high yield and high proanthocyanidin content in the product.

Description

technical field

[0001] The invention relates to a method for extracting proanthocyanidins from grape seeds with supercritical carbon dioxide, which belongs to the technology of extracting proanthocyanidins from grapes. Background technique

[0002] Proanthocyanidins are a general term for a large class of polyphenolic compounds that widely exist in the plant kingdom. They are condensed from different amounts of catechin or epicatechin, forming dimers to decamers. Proanthocyanidins have the ability to resist oxidation, scavenge free radicals, inhibit tumors, and resist mutations. They have cardiovascular activity and special effects on improving human microcirculation. They are widely used in food, medicine, health care products, and cosmetics.

[0003] Since the 1980s, a variety of proanthocyanidin preparations and functional cosmetics have been marketed and patented in the fields of medicine and cosmetics in foreign countries. They are widely used and have a bright future. ...

Examples

example 1

[0008] Example 1 Weigh 12.0 g of grape seed extract after oil removal and mix it with 12 mL of absolute ethanol, then put it into the extraction kettle, the temperature of the extraction kettle is 55 ° C, the pressure is 50 MPa, CO 2 Enter the extraction kettle through a high-pressure pump to ensure a 30-min extraction retention time, and then turn on the dynamic entrainer pump to continuously send absolute ethanol into the extraction kettle. The flow rate of the entrainer is 80mL / h, and the material is continuously discharged at the same time. The pressure of the first-stage separation tank is 10MPa. The temperature is 45°C, the pressure of the secondary separation tank is 5MPa, the temperature is 35°C, and the extraction time of the whole process is 1 hour. The obtained mixed solvent of proanthocyanidin and ethanol was evaporated and dried to obtain 1.9 g of proanthocyanidin product with a yield of 14.75%. The content of proanthocyanidin was 95.14% according to ultraviolet sp...

example 2

[0009] Example 2 Weigh 352g of the grape seed extract after oil removal and mix it with 535mL of absolute ethanol, then put it into the extraction kettle, the temperature of the extraction kettle is 45°C, the pressure is 40MPa, CO 2 Enter the extraction kettle through a high-pressure pump to ensure a 90min extraction retention time, and then turn on the dynamic entrainer pump to continuously send absolute ethanol into the extraction kettle. The flow rate of the entrainer is 120mL / h, and the material is continuously discharged at the same time. The pressure of the first-stage separation tank is 8MPa. The temperature is 45°C, the pressure of the secondary separation tank is 4MPa, the temperature is 35°C, and the extraction time of the whole process is 0.5 hours. The obtained proanthocyanidin and ethanol mixed solvent was evaporated and dried to obtain 51.5 g of proanthocyanidin product with a yield of 14.23%, and the proanthocyanidin content was 97.21% according to ultraviolet sp...

example 3

[0010] Example 3 Weigh 249g of the oil-removed grape seed extract and mix it with 440mL of absolute ethanol, then put it into the extraction kettle, the temperature of the extraction kettle is 35°C, the pressure is 30MPa, CO 2 Enter the extraction kettle through a high-pressure pump to ensure a 60-min extraction retention time, and then turn on the dynamic entrainer pump to continuously send absolute ethanol into the extraction kettle. The flow rate of the entrainer is 100mL / h, and the material is continuously discharged at the same time. The pressure of the first-stage separation tank is 6MPa. The temperature is 45°C, the pressure of the secondary separation tank is 5MPa, the temperature is 35°C, and the extraction time of the whole process is 0.5 hours. The obtained mixed solvent of proanthocyanidin and ethanol was evaporated and dried to obtain 34.0 g of proanthocyanidin product with a yield of 13.50%, and the content of proanthocyanidin was 98.91% according to ultraviolet s...

technical field

[0001] The invention relates to a method for extracting proanthocyanidins from grape seeds with supercritical carbon dioxide, which belongs to the technology of extracting proanthocyanidins from grapes. Background technique

[0002] Proanthocyanidins are a general term for a large class of polyphenolic compounds that widely exist in the plant kingdom. They are condensed from different amounts of catechin or epicatechin, forming dimers to decamers. Proanthocyanidins have the ability to resist oxidation, scavenge free radicals, inhibit tumors, and resist mutations. They have cardiovascular activity and special effects on improving human microcirculation. They are widely used in food, medicine, health care products, and cosmetics.

[0003] Since the 1980s, a variety of proanthocyanidin preparations and functional cosmetics have been marketed and patented in the fields of medicine and cosmetics in foreign countries. They are widely used and have a bright future. ...

Examples

example 1

[0008] Example 1 Weigh 12.0 g of grape seed extract after oil removal and mix it with 12 mL of absolute ethanol, then put it into the extraction kettle, the temperature of the extraction kettle is 55 ° C, the pressure is 50 MPa, CO 2 Enter the extraction kettle through a high-pressure pump to ensure a 30-min extraction retention time, and then turn on the dynamic entrainer pump to continuously send absolute ethanol into the extraction kettle. The flow rate of the entrainer is 80mL / h, and the material is continuously discharged at the same time. The pressure of the first-stage separation tank is 10MPa. The temperature is 45°C, the pressure of the secondary separation tank is 5MPa, the temperature is 35°C, and the extraction time of the whole process is 1 hour. The obtained mixed solvent of proanthocyanidin and ethanol was evaporated and dried to obtain 1.9 g of proanthocyanidin product with a yield of 14.75%. The content of proanthocyanidin was 95.14% according to ultraviolet sp...

example 2

[0009] Example 2 Weigh 352g of the grape seed extract after oil removal and mix it with 535mL of absolute ethanol, then put it into the extraction kettle, the temperature of the extraction kettle is 45°C, the pressure is 40MPa, CO 2 Enter the extraction kettle through a high-pressure pump to ensure a 90min extraction retention time, and then turn on the dynamic entrainer pump to continuously send absolute ethanol into the extraction kettle. The flow rate of the entrainer is 120mL / h, and the material is continuously discharged at the same time. The pressure of the first-stage separation tank is 8MPa. The temperature is 45°C, the pressure of the secondary separation tank is 4MPa, the temperature is 35°C, and the extraction time of the whole process is 0.5 hours. The obtained proanthocyanidin and ethanol mixed solvent was evaporated and dried to obtain 51.5 g of proanthocyanidin product with a yield of 14.23%, and the proanthocyanidin content was 97.21% according to ultraviolet sp...

example 3

[0010] Example 3 Weigh 249g of the oil-removed grape seed extract and mix it with 440mL of absolute ethanol, then put it into the extraction kettle, the temperature of the extraction kettle is 35°C, the pressure is 30MPa, CO 2 Enter the extraction kettle through a high-pressure pump to ensure a 60-min extraction retention time, and then turn on the dynamic entrainer pump to continuously send absolute ethanol into the extraction kettle. The flow rate of the entrainer is 100mL / h, and the material is continuously discharged at the same time. The pressure of the first-stage separation tank is 6MPa. The temperature is 45°C, the pressure of the secondary separation tank is 5MPa, the temperature is 35°C, and the extraction time of the whole process is 0.5 hours. The obtained mixed solvent of proanthocyanidin and ethanol was evaporated and dried to obtain 34.0 g of proanthocyanidin product with a yield of 13.50%, and the content of proanthocyanidin was 98.91% according to ultraviolet s...