The method of extracting 5-isopentenyl herbalin from water chestnut skin

A technology of isopentene and water chestnut skin, which is applied in the field of extracting and separating 5-isopentene-based herbalin, to meet the needs of the pharmaceutical industry, with high product purity and good separation effect

Active Publication Date: 2016-07-06
HEZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • The method of extracting 5-isopentenyl herbalin from water chestnut skin
  • The method of extracting 5-isopentenyl herbalin from water chestnut skin

Examples

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Embodiment 1

[0024] Add 8kg of fresh water chestnut skin powder into the extraction tank, add 32L of 70% by volume acetone aqueous solution each time, soak at 25°C for 24 hours, soak for 3 times in total, filter, combine the filtrates, concentrate under reduced pressure to obtain the extract 1.05 kg.

[0025] The extract was added to 5.0 L of water to make a turbid liquid, extracted three times with 5.0 L of ethyl acetate, the extracts were combined and concentrated under reduced pressure to obtain 120 g of the extract.

[0026] Add 300mL methanol to the extract to dissolve, mix the sample with 260g polyamide, volatilize the methanol to dryness, install the column, connect to the MCI column for medium pressure separation, use 40-100% by volume methanol aqueous solution as the mobile phase gradient elution, Collected in 500 mL portions, detected by thin-layer chromatography, collected the eluent with a combined mobile phase concentration of 70-90% by volume, and concentrated under reduced p...

Embodiment 2

[0030] Add 8kg of fresh water chestnut skin powder into the extraction tank, add 32L of 70% by volume acetone aqueous solution each time, soak at 25°C for 24 hours, soak for 3 times in total, filter, combine the filtrates, concentrate under reduced pressure to obtain the extract 1.05 kg.

[0031] The extract was added to 5.0 L of water to make a turbid liquid, extracted three times with 5.0 L of ethyl acetate, the extracts were combined and concentrated under reduced pressure to obtain 120 g of the extract.

[0032] Add 300mL methanol to the extract to dissolve, mix the sample with 260g polyamide, volatilize the methanol to dryness, install the column, connect to the MCI column for medium pressure separation, use 40-100% volume percent methanol aqueous solution as the mobile phase gradient elution, Collected in 500 mL portions, detected by thin-layer chromatography, collected the eluent with a combined mobile phase concentration of 70-90% by volume, and concentrated under redu...

Embodiment 3

[0036] Add 8kg of fresh water chestnut skin powder into the extraction tank, add 32L of 70% by volume acetone aqueous solution each time, soak at 25°C for 24 hours, soak for 3 times in total, filter, combine the filtrates, concentrate under reduced pressure to obtain the extract 1.05 kg.

[0037] The extract was added to 5.0 L of water to make a turbid liquid, extracted three times with 5.0 L of ethyl acetate, the extracts were combined and concentrated under reduced pressure to obtain 120 g of the extract.

[0038] Add 300mL methanol to the extract to dissolve, mix the sample with 260g polyamide, volatilize the methanol to dryness, install the column, connect to the MCI column for medium pressure separation, use 40-100% by volume methanol aqueous solution as the mobile phase gradient elution, Collected in 500 mL portions, detected by thin-layer chromatography, collected the eluent with a combined mobile phase concentration of 70-90% by volume, and concentrated under reduced p...

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Abstract

The invention relates to a method for extracting 5-isopentenyl aureusidin from eleocharis tuberose peels and belongs to the field of natural organic chemistry. The method is characterized by comprising the following steps of as an aqueous solution of acetone is used as a solvent, extracting the 5-isopentenyl aureusidin from the eleocharis tuberose peels to obtain an extract, extracting the extract with ethyl acetate to obtain an extractant, separating the extractant with a medium-pressure MCI column chromatography and a polyamide column chromatography to obtain a matter and repeatedly purifying the matter with a Sephadex LH-20 gel chromatography to obtain a 5-isopentenyl aureusidin product of which the content of the 5-isopentenyl aureusidin is above 95%. According to the method, a novel way for extracting and separating the 5-isopentenyl aureusidin from natural plants is created, the good separation effect is achieved, the product is high in purity, the eleocharis tuberose peels always regarded as wastes are changed into treasure, chromatographic materials, namely, MCI, polyamide and sol, can be repeatedly used, and the method has the advantages that raw materials are easily available, resources are abundant and the production cost is low; the product can be subjected to large-scale production and meets the needs of pharmaceutical industry.

Description

technical field [0001] The invention belongs to the field of natural organic chemistry, and relates to a method for extracting and separating 5-isopentenyl-rhetudin, in particular to a method for extracting and separating 5-isopentyl-arthoid from water chestnut skin. Background technique [0002] 5-Prenylaureusidin (5-Prenylaureusidin), the chemical name is 5-prenyl-4,6,3′,4′-tetrahydroxy aurone, it is an orange amorphous powder, soluble in methanol, Ethanol is a class of flavonoids that are less distributed in natural plants. It has been reported that 5-isopentenyl herthophyllin has good antioxidant, antifungal, antimicrobial, and glucose synthase inhibitory activities. 5-Isopentenyl herthophyllin can be isolated from plants, and can also be synthesized. The foreign patent WO97 / 26873 has disclosed its synthesis and antimicrobial research. The synthesis method published in this patent uses 2,4,6-trihydroxybenzene and 3,4-dimethoxybenzaldehyde as raw materials to synthesize...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/83
CPCC07D307/83
Inventor 罗杨合李行任刘珊方方韦家兴
Owner HEZHOU UNIV
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