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A kind of method for preparing high-purity isovitexin from Radix Grucoides

A technology of isovitexin and scorpion, which is applied in the field of preparation of isovitexin, can solve the problems of long time-consuming, many steps of silica gel column chromatography, low yield, etc., and achieve the effect of simple operation

Inactive Publication Date: 2011-12-14
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing methods for separating and purifying isovitexin are mainly traditional alcohol extraction and column chromatography purification, the extraction method takes a long time, the operation of silica gel column chromatography is complicated and has many steps, and the final extraction rate is not high
Homogenate extraction technology, macroporous adsorption resin enrichment technology and C18 reverse-phase medium-pressure silica gel column chromatography adopted in the Chinese patent "Method for Extracting and Purifying Vitexin and Isovitexin from Branches and Leaves of Pigeon Pea" (publication number CN101172991) Method, the separation and purification of isovitexin from pigeonpea is complex and time-consuming, and the yield is low
[0005] In summary, in the process of using plant resources to prepare isovitexin, the main factors restricting the extraction and separation of isovitexin are the backward extraction process, long time-consuming and complicated operation. Therefore, it is necessary to find a simple and safe method. , efficient and economical method for extracting and purifying isovitexin

Method used

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  • A kind of method for preparing high-purity isovitexin from Radix Grucoides
  • A kind of method for preparing high-purity isovitexin from Radix Grucoides
  • A kind of method for preparing high-purity isovitexin from Radix Grucoides

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Experimental program
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Effect test

Embodiment 1

[0030] (1) Grind 1000 grams of Chinese herbal medicine, add 20% methanol with a volume 10 times the mass of the medicinal material for ultrasonic extraction for 3 hours, filter, then add 20% methanol with a volume 10 times the mass of the medicinal material for ultrasonic extraction for 2 hours, and combine the two extractions after filtering solution, concentrated under reduced pressure to the extract to obtain A.

[0031] (2) Dissolve A completely in distilled water, extract it with ethyl acetate and n-butanol at a volume ratio of 1:1 until it is colorless, and concentrate the ethyl acetate extract to extract under reduced pressure to obtain B; The extract layer was concentrated under reduced pressure to obtain C.

[0032] (3) B and C are dissolved completely with 50% methanol respectively, cross a 0.45 μm microporous membrane, utilize methanol-0.4% glacial acetic acid (15: 85) as the mobile phase in the reversed-phase semi-preparative high performance liquid chromatography,...

Embodiment 2

[0034] (1), crush 1000 grams of Chinese herbal medicine, add 70% methanol with a volume of 10 times the mass of the medicinal material for ultrasonic extraction for 1 h, filter, then add 70% methanol with a volume of 8 times the mass of the medicinal material for ultrasonic extraction for 0.5 h, and combine the two after filtration The second extract was concentrated under reduced pressure to an extract to obtain A.

[0035] (2) Dissolve A completely in distilled water, extract it with ethyl acetate and n-butanol at a ratio of 1:1 until colorless, and concentrate the ethyl acetate extract to extract under reduced pressure to obtain B, n-butanol extract Concentrate under reduced pressure to obtain C.

[0036] (3), B and C are dissolved completely with 50% methanol, cross 0.45 μm microporous membrane, utilize methyl alcohol-0.4% glacial acetic acid (20: 80) as mobile phase in reversed-phase semi-preparative high performance liquid chromatography, chromatographic The column is a...

Embodiment 3

[0038] (1), crush 1000 grams of Chinese herbal medicine, add 35% methanol with a volume 8 times the mass of the medicinal material for ultrasonic extraction for 1 hour, filter, then add 35% methanol with a volume 8 times the mass of the medicinal material for ultrasonic extraction for 2 hours, filter and merge twice The extract was concentrated under reduced pressure to an extract to obtain A.

[0039] (2) Dissolve A completely in distilled water, extract it with ethyl acetate and n-butanol at a ratio of 1:1 until colorless, and concentrate the ethyl acetate extract to extract under reduced pressure to obtain B, n-butanol extract Concentrate under reduced pressure to obtain C.

[0040] (3), B and C are dissolved completely with 50% methanol, cross 0.45 μm microporous membrane, utilize methyl alcohol-0.4% glacial acetic acid (25: 75) as mobile phase in reversed-phase semi-preparative high performance liquid chromatography, chromatographic The column is a reversed-phase C-18 co...

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Abstract

The present invention relates to a method for preparing high-purity isovitexin from the herbal medicinal herb by using semi-preparative high-performance liquid chromatography. Ethyl ester and n-butanol were extracted until colorless, evaporated to dryness, dissolved in 50% methanol, and separated by reversed-phase semi-preparative high-efficiency liquid phase under certain chromatographic conditions. Fractions with the same retention time were collected and combined, and concentrated under reduced pressure. The isovitexin monomer with a purity of more than 98% can be obtained. The present invention uses only one chromatographic system to perform isocratic elution, can quickly separate high-purity isovitexin, produces less waste in the inventive method, occupies a small area, and has high column efficiency, and the method is simple and easy .

Description

technical field [0001] The invention relates to a method for preparing isovitexin, in particular to a method for preparing isovitexin with a purity of more than 98% from the medicinal material of scorpion. Background technique [0002] Thlaspi arvense (Thlaspi arvense.L) is the dry aboveground part of the cruciferous plant Thlaspi arvense. In Jiangsu, Gansu, Anhui and other places, it has the functions of clearing the liver and improving eyesight, harmonizing the middle and benefiting qi. It is mainly used to treat red eyes, swelling and pain, and tears. It is also commonly used to treat nephritis and endometritis. [0003] Isovitexin is the flavonoid component with the highest content in the medicinal materials of Grucoides. It belongs to carbon glycoside flavonoids, has a stable structure, is not easy to degrade, and has antioxidant and antibacterial activities. [0004] Retrieving domestic and foreign literature, only one report on the analysis of the volatile oil of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D407/04
Inventor 王立升庞赛史新段曼蒋敏捷
Owner GUANGXI UNIV
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