Process for extraction refining amygdalin

Abstract

The invention provides a process for extraction refining amygdalin which consists of, disintegrating the plant raw material containing rich bitter apricot seed into powder, removing the grease from the raw material powder by using CO2 as extracting agent, carrying out decompression segregation to the carbon dioxide containing vegetable fat, charging alcohol into ground-slag containing bitter apricot seed glycosides by the solid-to-liquid ratio of 1 : 3-10, agitating, filtering by suction to obtain the filter liquor, distilling and drying the filter liquor to obtain crude product of bitter apricot seed glycoside, dissolving the bitter apricot seed glycoside into ethanol, low temperature crystallizing, filtering and drying to obtain the high purity bitter apricot seed glycosides.

Description

technical field

[0001] The invention relates to a method for extracting the active ingredient amygdalin from plant raw materials, in particular to a separation and refining method for extracting amygdalin from horse egg fruit, plum seeds, almonds and peach kernels. technical background

[0002] Amygdalin is an aromatic cyanogenic glycoside, which exists in the seeds of Dafengzi Kema egg fruit, Rosaceae Plum, apricot and peach. Studies have found that amygdalin is an active ingredient in the treatment of respiratory diseases. It paralyzes and inhibits the respiratory central system by slowly releasing hydrocyanic acid in the body, thereby playing a role in relieving asthma. It is widely used in traditional Chinese medicine to treat cough etc. However, taking a large amount of bitter almonds and amygdalin can easily lead to severe poisoning. Amygdalin is hydrolyzed by amygdalin to produce prunin and amygdalin. Hydrocyanic acid reacts with the cytochrome enzyme ferric iron in...

Examples

example 1

[0021] Take the seeds of Plum, crush them into 10-40 meshes, weigh 200 grams of raw materials, put them in an extractor and pass them through supercritical CO 2 Deoiling after fluid extraction, extraction pressure 30MPa, extraction temperature 40°C, separation pressure 8MPa, separation temperature 50°C, after 4 hours, discharge the slag powder from the bottom of the extractor, add 1200ml of ethanol, and extract three times, each time 400 ml, combined the filtrates, recovered ethanol to an appropriate amount under reduced pressure, and vacuum-dried at 65° C. for 3 hours to obtain 11 g of a brownish-yellow extract, the content of which was determined to be 55% by HPLC.

[0022] Take 3 grams of the extracted extract, add a small amount of ethanol to dissolve and filter, then place it in a refrigerator at 4°C for 10 hours, and white crystals precipitate, filter, wash with a small amount of ethanol, and dry to obtain 1.3 grams. After HPLC detection, the content reaches 98.0% .

example 2

[0024] Take the seeds of Prunus mellifera, grind them into 20-40 mesh with a shear pulverizer, weigh 200 grams of raw materials, and put them in an extractor through supercritical CO 2 Deoiling after fluid extraction, extraction pressure 20MPa, extraction temperature 60°C, separation pressure 9MPa, separation temperature 70°C, after 6 hours, discharge the slag powder from the bottom of the extractor, add 1200ml of ethanol, and extract three times, each time 400 ml, combined the filtrates, recovered ethanol to an appropriate amount under reduced pressure, and dried in vacuo at 65°C for 3 hours to obtain 12 g of a brownish-yellow extract, the content of which was determined by HPLC to be 50%.

[0025] 4 g of the extracted extract was dissolved by adding a small amount of ethanol sonicated, then stood still at room temperature for 1 hour, filtered to obtain white crystals, and dried to obtain 1.6 g. The content reached 92.3% through HPLC detection.

example 3

[0027] Take the seeds of bitter almonds, grind them into 20-40 meshes with a shearing mill, weigh 200 grams of raw materials, and put them in an extractor through supercritical CO 2 Deoiling after fluid extraction, extraction pressure 32MPa, extraction temperature 50°C, separation pressure 5Mpa, separation temperature 30°C, after 4 hours, discharge the slag powder from the bottom of the extractor, add 1500ml of ethanol, and extract three times, each time 500 ml, combined the filtrates, recovered ethanol to an appropriate amount under reduced pressure, and vacuum-dried at 65° C. for 3 hours to obtain 5.5 g of brown-yellow extract, the content of which was 60% as determined by HPLC.

[0028] Take 4 grams of the extracted extract, add a small amount of ethanol to dissolve and filter, then place it at 4 ° C for 10 hours, precipitate white crystals, filter, wash with a small amount of ethanol, and dry to obtain 1.8 grams. After HPLC detection, the content reaches 95.4%.

technical field

[0001] The invention relates to a method for extracting the active ingredient amygdalin from plant raw materials, in particular to a separation and refining method for extracting amygdalin from horse egg fruit, plum seeds, almonds and peach kernels. technical background

[0002] Amygdalin is an aromatic cyanogenic glycoside, which exists in the seeds of Dafengzi Kema egg fruit, Rosaceae Plum, apricot and peach. Studies have found that amygdalin is an active ingredient in the treatment of respiratory diseases. It paralyzes and inhibits the respiratory central system by slowly releasing hydrocyanic acid in the body, thereby playing a role in relieving asthma. It is widely used in traditional Chinese medicine to treat cough etc. However, taking a large amount of bitter almonds and amygdalin can easily lead to severe poisoning. Amygdalin is hydrolyzed by amygdalin to produce prunin and amygdalin. Hydrocyanic acid reacts with the cytochrome enzyme ferric iron in...

Examples

example 1

[0021] Take the seeds of Plum, crush them into 10-40 meshes, weigh 200 grams of raw materials, put them in an extractor and pass them through supercritical CO 2 Deoiling after fluid extraction, extraction pressure 30MPa, extraction temperature 40°C, separation pressure 8MPa, separation temperature 50°C, after 4 hours, discharge the slag powder from the bottom of the extractor, add 1200ml of ethanol, and extract three times, each time 400 ml, combined the filtrates, recovered ethanol to an appropriate amount under reduced pressure, and vacuum-dried at 65° C. for 3 hours to obtain 11 g of a brownish-yellow extract, the content of which was determined to be 55% by HPLC.

[0022] Take 3 grams of the extracted extract, add a small amount of ethanol to dissolve and filter, then place it in a refrigerator at 4°C for 10 hours, and white crystals precipitate, filter, wash with a small amount of ethanol, and dry to obtain 1.3 grams. After HPLC detection, the content reaches 98.0% .

example 2

[0024] Take the seeds of Prunus mellifera, grind them into 20-40 mesh with a shear pulverizer, weigh 200 grams of raw materials, and put them in an extractor through supercritical CO 2 Deoiling after fluid extraction, extraction pressure 20MPa, extraction temperature 60°C, separation pressure 9MPa, separation temperature 70°C, after 6 hours, discharge the slag powder from the bottom of the extractor, add 1200ml of ethanol, and extract three times, each time 400 ml, combined the filtrates, recovered ethanol to an appropriate amount under reduced pressure, and dried in vacuo at 65°C for 3 hours to obtain 12 g of a brownish-yellow extract, the content of which was determined by HPLC to be 50%.

[0025] 4 g of the extracted extract was dissolved by adding a small amount of ethanol sonicated, then stood still at room temperature for 1 hour, filtered to obtain white crystals, and dried to obtain 1.6 g. The content reached 92.3% through HPLC detection.

example 3

[0027] Take the seeds of bitter almonds, grind them into 20-40 meshes with a shearing mill, weigh 200 grams of raw materials, and put them in an extractor through supercritical CO 2 Deoiling after fluid extraction, extraction pressure 32MPa, extraction temperature 50°C, separation pressure 5Mpa, separation temperature 30°C, after 4 hours, discharge the slag powder from the bottom of the extractor, add 1500ml of ethanol, and extract three times, each time 500 ml, combined the filtrates, recovered ethanol to an appropriate amount under reduced pressure, and vacuum-dried at 65° C. for 3 hours to obtain 5.5 g of brown-yellow extract, the content of which was 60% as determined by HPLC.

[0028] Take 4 grams of the extracted extract, add a small amount of ethanol to dissolve and filter, then place it at 4 ° C for 10 hours, precipitate white crystals, filter, wash with a small amount of ethanol, and dry to obtain 1.8 grams. After HPLC detection, the content reaches 95.4%.