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Method for preparing high-purity scutellarin

A technology of scutellarin B and scutellarin, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve a large number of problems such as acid and alkali, environmental pollution, and low yield, and achieve production costs Low cost, low price, high yield effect

Active Publication Date: 2010-06-23
CHENGDU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purity can reach more than 98%, but the above patents need a large amount of acid and alkali to realize, which brings great pollution to the environment, and the yield is low, and there are many problems in industrialization promotion

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Weigh 10Kg of ethylenediamine, 15Kg of methyl acrylate, and 10Kg of polyamide resin, and put them in a reaction tank with a stirring speed of 50 rpm, a reaction temperature of 25°C, and a reaction time of 24 hours, then filter, wash with ethanol, and dry to obtain 15Kg of modified polyamide resin , as a chromatographic material.

[0030] Weigh 100g of commercially available scutellarin, wherein the content of scutellarin B is 85% by weight, add 500ml of boiling water and stir evenly, adjust the pH value to 7 with 20% by weight sodium carbonate solution, dissolve, filter, and add the filtrate On the chromatographic material column, use deionized water as the eluent, collect the eluent in parts, combine the eluent whose purity is greater than 98% by weight, add a hydrochloric acid solution with a concentration of 10% by weight, and adjust the pH to 2. Stand still for 2 hours, filter the precipitate, wash with water until neutral, and dry at 80°C to obtain 58.2g of scutell...

Embodiment 2

[0032] Weigh 10Kg of ethylenediamine, 20Kg of methyl acrylate, and 10Kg of polyamide resin, and put them in a reaction tank with a stirring speed of 50 rpm, a reaction temperature of 25°C, and a reaction time of 24 hours, then filter, wash with ethanol, and dry to obtain 17Kg of modified polyamide resin .

[0033] Weigh 100g of commercially available scutellarin, wherein the content of scutellarin B is 85% by weight, add 500ml of boiling water and stir evenly, adjust the pH value to 7 with 10% by weight of ammonia water, dissolve, filter, and add the filtrate to the layer Analyze the material on the column, use deionization as the eluent, collect in parts, combine the eluent whose purity is greater than 98%, add a hydrochloric acid solution with a concentration of 10% by weight, adjust the pH to 2, let it stand for 2 hours, filter The precipitate was taken, washed with water until neutral, and dried at 80° C. to obtain 56.5 g of scutellarin, with a content of 98.7% by weight. ...

Embodiment 3

[0035] Weigh 10Kg of ethylenediamine, 30Kg of methyl acrylate, and 15Kg of polyamide resin, and place them in a reaction tank with a stirring speed of 50 rpm, a reaction temperature of 25°C, and a reaction time of 24 hours, then filter, wash with ethanol, and dry to obtain 20Kg of modified polyamide resin .

[0036] Weigh 500g of commercially available scutellarin, wherein the content of scutellarin B is 85% by weight, add 2500ml of boiling water and stir evenly, adjust the pH value to 7 with 20% by weight sodium carbonate solution to dissolve scutellarin, Filtrate, add the filtrate to the chromatographic material column, use deionization as the eluent, collect in parts, combine the eluent whose purity is greater than 98% by weight, add hydrochloric acid solution with a concentration of 10% by weight, and adjust the pH to 2, let stand for 2 hours, filter the precipitate, wash with water until neutral, and dry at 80°C to obtain 256.7g of scutellarin with a content of 98.4% by w...

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PUM

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Abstract

The invention provides a method for preparing high-purity scutellarin, which solves the problem that the prior preparation method is high in pollution, low in yield and high in cost. The method comprises the following: (1) a dissolution step, which is to take commercially available breviscapinun of which the scutellarin content in percentage by weight is 85 percent, dissolve the breviscapinun in alkaline water which is 5 to 10 times the weight of the breviscapinun and has a pH of 7 to 9 and filter the obtained product, and (2) a separation step, which is to use chromatography material to perform column chromatography on filtrate of which the sample loading amount is 1:1-3, elute the obtained product with elution water 8 to 10 times the volume of a column, collect the obtained product part by part, combine eluent of which the purity is greater than weight percentage by 98 percent, regulate pH to 2, precipitate, stand and filter the obtained product, wash precipitate with deionized water to be neutral, dry the obtained product and obtain the high-purity scutellarin.

Description

Technical field: [0001] The present invention is related to the preparation of high-purity plant raw materials. Background technique [0002] Erigeron breviscapus (Vant)}land.Mazz is the dry whole plant of Compositae, also known as Erigeron breviscapus, distributed in Yunnan, Sichuan, Guizhou, Guangxi, Hunan and other places. This product is cold in nature, slightly bitter, and has the effects of dispelling cold and relieving the exterior, expelling wind and dampness, promoting blood circulation and removing blood stasis, dredging meridian and activating collaterals, reducing inflammation and relieving pain. Breviscapine is an active ingredient of flavonoids extracted from breviscapine herb, mainly scutellarin B, also known as scutellarin, and its chemical name is 4', 5, 6-trihydroxyflavone-7-O- Glucuronide, the raw material drug of breviscapine purchased from the market at present, is analyzed by HPLC, and the content of scutellarin B is between 80-90%. It is widely used c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08
Inventor 邓小宽何正有杨放
Owner CHENGDU UNIV
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