Method for comprehensively extracting and purifying oxidation-resistant active ingredient in sugarcane toppers or slag

Abstract

The invention discloses a method for comprehensively extracting and purifying anthocyanin and general flavone which does not comprise the anthocyanin in sugarcane toppers or slag. The method comprises the steps of firstly extracting the sugarcane toppers or slag by an organic solvent, concentrating the extract and passing the extract through a chromatographic column filled with a macro-porous adsorptive resin, removing water-soluble impurities such as glucide by a gradient elution method, respectively collecting the ethanol eluent with a low concentration and the ethanol eluent with a high concentration to obtain two ingredients of the anthocyanin and the general flavone which does not comprise the anthocyanin, and respectively enriching and purifying the ingredients of the anthocyanin and the general flavone which does not comprise the anthocyanin by a solvent extraction method and an acid and alkali treatment method so as to obtain the anthocyanin and the general flavone which does not comprise the anthocyanin. Compared with the reported methods for extraction and separation of similar ingredients, the method of the invention can not only completely extract two main oxidation-resistant ingredients in the sugarcane toppers or slag, also the reagents consumed in the technological process can be recycled. The method has low production cost, high purity and mature technology, and is easily controlled and in favour of industrial production.

Description

technical field

[0001] The invention belongs to the technical field of methods for comprehensively extracting, separating and purifying main antioxidant active ingredients in sugarcane tip or bagasse, and specifically relates to a method for comprehensively extracting and purifying main antioxidant active ingredients in sugarcane tip or bagasse—total flavonoids and anthocyanins . Background technique

[0002] Sugarcane (Saccharum officenarum L.) is a plant of the genus Saccharum in the Gramineae family. It is native to tropical and subtropical regions. It has a high light saturation point, low carbon dioxide compensation point, low photorespiration rate, and high photosynthetic intensity. 90% of the planting area of ​​sugarcane is distributed in Between the Tropic of Cancer and the South. my country is the earliest country in the world to grow sugar cane, with a history of about 2,500 years. Sugar cane has a high biological yield and a large profit, and is the main raw mate...

Examples

Embodiment 1

[0024] 100 g of chopped sugarcane tip raw material was extracted twice with 60% ethanol with a solid-to-liquid ratio of 1:15 (mass to volume ratio) for 1 hour each time. Next, the raw material extract is passed through a chromatographic column filled with D101 macroporous adsorption resin, sugar and other water-soluble impurities are washed away with pure water, and then gradient elution is performed using ethanol aqueous solution with a concentration of 10-100% by volume. Collect the eluate with a concentration of 60% by volume, concentrate, use sodium hydroxide solution to adjust the pH value of the concentrated eluate to 10, use 3 times the volume of ethyl acetate to extract twice, and partially wash the sodium hydroxide solution with hydrochloric acid Adjust the pH value to 6, then extract twice with 3 times the volume of ethyl acetate, wash with water until neutral, then evaporate and concentrate under reduced pressure, freeze-dry, and determine the total flavonoids by cal...

Embodiment 2

[0026] 100 g of the extracted bagasse raw material was ultrasonically extracted 4 times with 60% methanol at a solid-to-liquid ratio of 1:6 (mass to volume ratio), 1 hour each time. Next, the raw material extract is passed through a chromatographic column filled with D301 macroporous adsorption resin, sugar and other water-soluble impurities are washed off with pure water, and then gradient elution is performed using ethanol aqueous solution with a concentration of 10-100% by volume. Collect the eluate with a volume percentage concentration of 70%, concentrate, use potassium hydroxide solution to adjust the pH value of the concentrated eluate to 9, use 1 volume of n-butanol to extract twice, and partially wash the potassium hydroxide solution with acetic acid Adjust the pH value to 5, then extract 3 times with 2 times the volume of n-butanol, wash with water to neutrality, then evaporate and concentrate under reduced pressure, freeze-dry, and determine the total flavonoids by c...

Embodiment 3

[0028] 100 g of chopped sugarcane tip raw material was extracted 3 times by percolation with 80% ethanol at a solid-to-liquid ratio of 1:8 (mass to volume ratio), 1 hour each time. Then, the raw material extract is passed through a chromatographic column filled with AB-8 macroporous adsorption resin, sugar and other water-soluble impurities are washed off with pure water, and then gradient washing is carried out with an ethanol aqueous solution with a concentration of 10 to 100% by volume. take off. Collect the eluate with a volume percentage concentration of 80%, concentrate, use sodium carbonate solution to adjust the pH value of the concentrated eluate to 9, use 2 times the volume of n-butanol to extract 3 times, and adjust the sodium carbonate solution part with formic acid to The pH value is 4, and then extracted 4 times with 1 times the volume of ethyl acetate, washed with water until neutral, then concentrated by evaporation under reduced pressure, freeze-dried, and det...

technical field

[0001] The invention belongs to the technical field of methods for comprehensively extracting, separating and purifying main antioxidant active ingredients in sugarcane tip or bagasse, and specifically relates to a method for comprehensively extracting and purifying main antioxidant active ingredients in sugarcane tip or bagasse—total flavonoids and anthocyanins . Background technique

[0002] Sugarcane (Saccharum officenarum L.) is a plant of the genus Saccharum in the Gramineae family. It is native to tropical and subtropical regions. It has a high light saturation point, low carbon dioxide compensation point, low photorespiration rate, and high photosynthetic intensity. 90% of the planting area of ​​sugarcane is distributed in Between the Tropic of Cancer and the South. my country is the earliest country in the world to grow sugar cane, with a history of about 2,500 years. Sugar cane has a high biological yield and a large profit, and is the main raw mate...

Examples

Embodiment 1

[0024] 100 g of chopped sugarcane tip raw material was extracted twice with 60% ethanol with a solid-to-liquid ratio of 1:15 (mass to volume ratio) for 1 hour each time. Next, the raw material extract is passed through a chromatographic column filled with D101 macroporous adsorption resin, sugar and other water-soluble impurities are washed away with pure water, and then gradient elution is performed using ethanol aqueous solution with a concentration of 10-100% by volume. Collect the eluate with a concentration of 60% by volume, concentrate, use sodium hydroxide solution to adjust the pH value of the concentrated eluate to 10, use 3 times the volume of ethyl acetate to extract twice, and partially wash the sodium hydroxide solution with hydrochloric acid Adjust the pH value to 6, then extract twice with 3 times the volume of ethyl acetate, wash with water until neutral, then evaporate and concentrate under reduced pressure, freeze-dry, and determine the total flavonoids by cal...

Embodiment 2

[0026] 100 g of the extracted bagasse raw material was ultrasonically extracted 4 times with 60% methanol at a solid-to-liquid ratio of 1:6 (mass to volume ratio), 1 hour each time. Next, the raw material extract is passed through a chromatographic column filled with D301 macroporous adsorption resin, sugar and other water-soluble impurities are washed off with pure water, and then gradient elution is performed using ethanol aqueous solution with a concentration of 10-100% by volume. Collect the eluate with a volume percentage concentration of 70%, concentrate, use potassium hydroxide solution to adjust the pH value of the concentrated eluate to 9, use 1 volume of n-butanol to extract twice, and partially wash the potassium hydroxide solution with acetic acid Adjust the pH value to 5, then extract 3 times with 2 times the volume of n-butanol, wash with water to neutrality, then evaporate and concentrate under reduced pressure, freeze-dry, and determine the total flavonoids by c...

Embodiment 3

[0028] 100 g of chopped sugarcane tip raw material was extracted 3 times by percolation with 80% ethanol at a solid-to-liquid ratio of 1:8 (mass to volume ratio), 1 hour each time. Then, the raw material extract is passed through a chromatographic column filled with AB-8 macroporous adsorption resin, sugar and other water-soluble impurities are washed off with pure water, and then gradient washing is carried out with an ethanol aqueous solution with a concentration of 10 to 100% by volume. take off. Collect the eluate with a volume percentage concentration of 80%, concentrate, use sodium carbonate solution to adjust the pH value of the concentrated eluate to 9, use 2 times the volume of n-butanol to extract 3 times, and adjust the sodium carbonate solution part with formic acid to The pH value is 4, and then extracted 4 times with 1 times the volume of ethyl acetate, washed with water until neutral, then concentrated by evaporation under reduced pressure, freeze-dried, and det...