Method for extracting apigenin from Chinese violet

Abstract

The invention provides a method for extracting apigenin from Chinese violet, which greatly improves the yield and the purity of the apiolin. A set of following procedures is provided for extracting and separating high-purity apiolin from the Chinese violet: processing ultrasonically while adopting alcohol extract, centrifugating, concentrating, extracting, performing adsorption chromatography by using macroporous absorption resin LSA-10 and chromatographic column silica gel, continuously separating, concentrating, and crystallizing by acetone to obtain the pure apigenin. The integral separation process has low requirement on environment conditions, the separation time is shorter and the purity is high. Separating materials are easy to obtain and cheap, the separation operation process is simple and easy to control, and the purifying efficiency is high by adopting crystallization and recrystallization.

Description

technical field

[0001] The present invention relates to the comprehensive utilization of medicinal plants such as Viola chinensis. More specifically, the present invention provides a method for extracting apigenin from Viola chinensis, which greatly improves the yield and purity of apigenin. Therefore, the present invention belongs to The field of extracting biological products from medicinal plants such as violadin. Background technique

[0002] Apigenin is a naturally occurring flavonoid compound known as "phytoestrogen" and has strong biological activity. Apigenin exists in many plants in the form of plant yellow pigment. The pure product is yellow powder, odorless and tasteless. Is a natural antioxidant. The chemical name is 5,7,4'-trihydroxyflavone, the molecular formula and molecular weight are C 15 h 10 o 5 And 270.25, melting point 347.5 ° C, almost insoluble in water, slightly soluble in hot alcohol, soluble in dilute KOH solution.

[0003] Studies have shown ...

Examples

Embodiment 1

[0032] Weigh 500kg of viola powder, add 70% methanol 4000L, ultrasonicate at 50°C for 10min, extract for 30min and then centrifuge for 10min (3000r / min), the precipitate is extracted once with 70% methanol 1000L, and the two supernatants are combined liquid. Concentrate the supernatant to about 100L, add 40L of petroleum ether to the concentrated solution for extraction, remove the lower layer, extract the concentrated solution four times continuously, combine the four lower layer extracts for a total of 160L, and then use ethyl acetate 40L The solution containing petroleum ether was extracted, and after the solution containing petroleum ether was continuously extracted four times, the ethyl acetate part of the upper layer was combined for a total of 160L, and the extract was concentrated to obtain ethyl acetate concentrate, which was stored in a fume hood Dry at 60°C. Completely dissolve ethyl acetate in 10 L of 50% ethanol at 40°C, extract and dry the product, put it on a m...

Embodiment 2

[0038] Weigh 1000kg of viola powder, add 70% methanol 8000L, ultrasonically treat at 50°C for 10min, extract for 30min and then centrifuge for 10min (3000r / min), extract the precipitate once with 70% methanol 2000L, and combine the two supernatants liquid. Concentrate the supernatant to about 200L, add petroleum ether 80L to the concentrated solution for extraction, remove the lower layer, extract the concentrated solution four times continuously, combine the four lower layer extracts for a total of 320L, and then use ethyl acetate 80L The solution containing petroleum ether was extracted, and after the solution containing petroleum ether was continuously extracted four times, the ethyl acetate part of the upper layer was combined for a total of 320L, and the extract was concentrated to obtain ethyl acetate concentrate, which was stored in a fume hood Dry at 60°C. Completely dissolve ethyl acetate in 20 L of 50% ethanol at 40°C, extract and dry the product, put it on a macrop...

Embodiment 3

[0040] Weigh 300kg of viola powder, add 2000L of 70% ethanol, ultrasonicate for 10min at 50°C, extract for 30min and then centrifuge for 10min (3000r / min), extract the precipitate once with 1000L of 70% ethanol, and combine the two supernatants liquid. Concentrate the supernatant to about 50L, add petroleum ether 30L to the concentrated solution for extraction, remove the lower layer, extract the concentrated solution four times continuously, combine the four lower layer extracts for a total of 120L, and then use ethyl acetate 30L The solution containing petroleum ether is extracted, and after the solution containing petroleum ether is continuously extracted four times, the ethyl acetate part of the upper layer is combined for a total of 120L, and the extract is concentrated to obtain ethyl acetate concentrate. Dry at 60°C. Completely dissolve ethyl acetate in 10 L of 50% ethanol at 40°C, extract and dry the product, put it on a macroporous adsorption resin LSA-10 column, and...

technical field

[0001] The present invention relates to the comprehensive utilization of medicinal plants such as Viola chinensis. More specifically, the present invention provides a method for extracting apigenin from Viola chinensis, which greatly improves the yield and purity of apigenin. Therefore, the present invention belongs to The field of extracting biological products from medicinal plants such as violadin. Background technique

[0002] Apigenin is a naturally occurring flavonoid compound known as "phytoestrogen" and has strong biological activity. Apigenin exists in many plants in the form of plant yellow pigment. The pure product is yellow powder, odorless and tasteless. Is a natural antioxidant. The chemical name is 5,7,4'-trihydroxyflavone, the molecular formula and molecular weight are C 15 h 10 o 5 And 270.25, melting point 347.5 ° C, almost insoluble in water, slightly soluble in hot alcohol, soluble in dilute KOH solution.

[0003] Studies have shown ...

Examples

Embodiment 1

[0032] Weigh 500kg of viola powder, add 70% methanol 4000L, ultrasonicate at 50°C for 10min, extract for 30min and then centrifuge for 10min (3000r / min), the precipitate is extracted once with 70% methanol 1000L, and the two supernatants are combined liquid. Concentrate the supernatant to about 100L, add 40L of petroleum ether to the concentrated solution for extraction, remove the lower layer, extract the concentrated solution four times continuously, combine the four lower layer extracts for a total of 160L, and then use ethyl acetate 40L The solution containing petroleum ether was extracted, and after the solution containing petroleum ether was continuously extracted four times, the ethyl acetate part of the upper layer was combined for a total of 160L, and the extract was concentrated to obtain ethyl acetate concentrate, which was stored in a fume hood Dry at 60°C. Completely dissolve ethyl acetate in 10 L of 50% ethanol at 40°C, extract and dry the product, put it on a m...

Embodiment 2

[0038] Weigh 1000kg of viola powder, add 70% methanol 8000L, ultrasonically treat at 50°C for 10min, extract for 30min and then centrifuge for 10min (3000r / min), extract the precipitate once with 70% methanol 2000L, and combine the two supernatants liquid. Concentrate the supernatant to about 200L, add petroleum ether 80L to the concentrated solution for extraction, remove the lower layer, extract the concentrated solution four times continuously, combine the four lower layer extracts for a total of 320L, and then use ethyl acetate 80L The solution containing petroleum ether was extracted, and after the solution containing petroleum ether was continuously extracted four times, the ethyl acetate part of the upper layer was combined for a total of 320L, and the extract was concentrated to obtain ethyl acetate concentrate, which was stored in a fume hood Dry at 60°C. Completely dissolve ethyl acetate in 20 L of 50% ethanol at 40°C, extract and dry the product, put it on a macrop...

Embodiment 3

[0040] Weigh 300kg of viola powder, add 2000L of 70% ethanol, ultrasonicate for 10min at 50°C, extract for 30min and then centrifuge for 10min (3000r / min), extract the precipitate once with 1000L of 70% ethanol, and combine the two supernatants liquid. Concentrate the supernatant to about 50L, add petroleum ether 30L to the concentrated solution for extraction, remove the lower layer, extract the concentrated solution four times continuously, combine the four lower layer extracts for a total of 120L, and then use ethyl acetate 30L The solution containing petroleum ether is extracted, and after the solution containing petroleum ether is continuously extracted four times, the ethyl acetate part of the upper layer is combined for a total of 120L, and the extract is concentrated to obtain ethyl acetate concentrate. Dry at 60°C. Completely dissolve ethyl acetate in 10 L of 50% ethanol at 40°C, extract and dry the product, put it on a macroporous adsorption resin LSA-10 column, and...

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