Luteolin metal salt and its preparation method and use

A technology of luteolin and metal salts, which is applied in the direction of pharmaceutical formulations, medical preparations containing active ingredients, respiratory diseases, etc., can solve the problems of low extraction rate of natural products, poor water solubility, and impact on application, and achieve prevention or treatment Hepatic fibrosis, easy operation, low cost effect

Inactive Publication Date: 2004-05-05
HANGZHOU FST PHARMA
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  • Description
  • Claims
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Problems solved by technology

However, due to the low extraction rate of natural products and poor wate

Method used

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  • Luteolin metal salt and its preparation method and use
  • Luteolin metal salt and its preparation method and use

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preparation example Construction

[0011] The specific steps of the preparation method of luteolin metal salt are as follows:

[0012] 1) Add 100 to 200 grams of rutin and 141 to 200 grams of sodium hydroxide in 3.5 to 4.5 liters of water in a 5L three-necked bottle, heat, reflux for 12 to 20 hours and cool to room temperature, and slowly add 500 to 600 ml of concentrated Hydrochloric acid to pH=1~4, suction filtration, obtain light yellow solid, solid product is joined in the water of 1000~1500 milliliters, is that 10~20% sodium hydroxide is adjusted pH=11~14 with weight percentage, filter cooling, use Adjust the pH to 1-4 with 10-20% hydrochloric acid by weight, filter, and dry the crude product at 80-100°C;

[0013] 2) Add the crude product to a 1:1 mixture of water and methanol, heat to dissolve, add 2 to 4 grams of activated carbon, reflux for 10 to 30 minutes, filter while it is hot, slowly cool the filtrate to room temperature, and keep it warm for 3 to 6 hours , filter, wash the filter cake with methan...

Embodiment 1

[0016] 1). Add 100 grams (0.164 moles) of rutin and 141 grams (3.53 moles) of sodium hydroxide to 4.5 liters of water in a 5-liter three-necked bottle, heat, reflux for 12 hours and cool to room temperature, then slowly add 560 milliliters of concentrated hydrochloric acid To pH = 1-4, filter with suction to obtain light yellow solid. The reaction formula is:

[0017]

[0018] The solid product was added to 1000 ml of water. Adjust pH=11-14 with 10% sodium hydroxide, filter and cool, adjust to pH=1-4 with 10% hydrochloric acid, and filter. After drying at 80°C, 41.0 g of crude product was obtained, and the calculated yield was 87.6%;

[0019] 2) Add 41.0 grams of crude product into a mixed solution of 123 grams of water and 123 grams of methanol, heat to dissolve, add 2 grams of gac, and reflux for 10 minutes. Filtrate while hot, slowly cool the filtrate to room temperature, keep warm for 3 hours, filter, wash the filter cake with methanol, and drain once. 26.7 grams of...

Embodiment 2

[0024] 1) Add 200 grams of rutin and 200 grams of sodium hydroxide to 4.5 liters of water in a 5-liter three-necked bottle, heat, reflux for 20 hours and cool to room temperature, slowly add 600 milliliters of concentrated hydrochloric acid to pH=4, and suction filter to obtain Light yellow solid, the solid product was added to 1500 ml of water, adjusted to pH=14 with 20% by weight sodium hydroxide, filtered and cooled, adjusted to pH=4 with 20% by weight of hydrochloric acid, filtered, and baked at 100°C Dried crude product;

[0025] 2) Add the crude product to a 1:1 mixture of water and methanol, heat to dissolve, add 4 grams of activated carbon, reflux for 30 minutes, filter while it is hot, slowly cool the filtrate to room temperature, keep it warm for 6 hours, filter, and wash with methanol The filter cake is drained once, dried and refined at 100°C;

[0026] 3) Get 3 grams of sodium metal in 200 milliliters of absolute ethanol to make a sodium ethylate solution, put 15 ...

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Abstract

A luteolin-metal salt for preventing and treating pulmonary fibrosis is prepared through adding rutin to the aqueous solution of sodium hydroxide, thermal reflux, cooling, regulating pH=1-4, filtering to obtain yellow solid, dissolving it in water, regulating pH=11-14, filtering, regulating pH=1-4, filtering, baking to obtain coarse product, refining in the mixture of water and methanol by heating, adding it to the solution of Na in absolute alcohol, reacting, and vacuum concentrating until it become solid. Its advantages are high purity and output rate, and low cost.

Description

technical field [0001] The invention relates to a metal salt of luteolin and its preparation method and application. Background technique [0002] Luteolin, also known as luteolin, is an active ingredient isolated from plants such as Prunella vulgaris, Chenpi, and true chrysanthemum. There have been many patent reports in China to obtain luteolin by plant extraction. Its natural products have been used in clinical treatment of cough and expectorant and have good curative effect. However, due to the low extraction rate of natural products and poor water solubility, the clinical application of this product has been greatly affected. Contents of the invention [0003] The object of the present invention is to provide a metal salt of luteolin and its preparation method and application. [0004] The structural formula of luteolin metal salt is: Wherein R1, R2, R3, R4 represent -OH or -ONa, -OK active metal oxygen groups. ...

Claims

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Application Information

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IPC IPC(8): A61K31/352A61P11/00A61P31/14C07D311/30
Inventor 潘建林王玉伟徐竹清陈长荣吴永龙
Owner HANGZHOU FST PHARMA
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