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Process for preparing high purity scutellarin raw materials

A technology of scutellarin and preparation process, which is applied in the field of preparation technology of raw materials, can solve the problems of improving the purity of unreported scutellarin and eliminating side effects, achieves easy industrial production, reduces toxicity, and solves instability sexual effect

Active Publication Date: 2006-10-04
KUNMING LONGJIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no report on the refining process of scutellarin in the relevant literature and patent materials, and there is no report on the improvement of the purity of scutellarin and the elimination of side effects

Method used

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  • Process for preparing high purity scutellarin raw materials

Examples

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Embodiment 1

[0021] Weigh 1000g of commercially available breviscapine crude drug, add 10 times the weight of water, adjust the pH value to 7 with 30% benzene disodium phosphate solution, make it completely dissolved, filter, add 8 times of acetone to the filtrate at 25°C for precipitation, and Stir while adding to make the precipitation complete, let it stand for 12 hours, filter, add acetone to wash three times, then move the precipitate to another container, add 6 times the amount of 40% acetone, stir well, then add 25% hydrochloric acid to adjust the acidity PH1-2, let stand for 10 hours, filter with suction, wash with water until neutral, wash once with ethanol, and dry to obtain refined scutellarin. The content of scutellarin by HPLC analysis is 99.5861%, as shown in the attached drawing Show.

Embodiment 2

[0023] Weigh 1000g of commercially available scutellarin raw material, add 15 times the weight of water, adjust the pH value to 7 with 20% sodium ethoxide solution, dissolve completely, filter, add 10 times of acetone to the filtrate at 25°C for precipitation, add as you go Stir to make the precipitation complete, let stand for 12 hours, filter, add acetone to wash three times, then move the precipitate to another container, add 6 times the amount of 40% acetone, stir well, then add 25% hydrochloric acid to adjust the acidity to PH1 -2, let stand for 10 hours, filter with suction, wash with water until neutral, then wash with ethanol once. The obtained product is repeated 2-3 times according to the above operation method, and dried to obtain refined scutellarin.

[0024] Detection method: chromatographic conditions and system suitability test (using octadecyl bonded silica gel as filler: methanol-0.1% phosphoric acid solution (40:60) is mobile phase; detection wavelength is 33...

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Abstract

The related preparation method for high-pure scutellarin drug comprises: 1. adding 200wt% water into container with material and alkaline solution (pH > 9) to adjust liquid to pH value as 4-8 for complete dissolution; 2. adding solvent with weight more than 3 times at 18-35Deg, depositing, keeping static, filtering, and cleaning precipitum with solvent; 3. transferring precipitum into solvent with 10-60wt% solvent, adjusting pH to 1-2 with acid, depositing, filtering, cleaning with water to neutrality, and drying to obtain the final product.

Description

technical field [0001] The invention relates to a preparation process of a bulk drug in the pharmaceutical industry, in particular to a preparation process of a high-purity bulk drug. Background technique [0002] Erigeron breviscapus (Vant.) Hand-Mazz is a flavonoid active ingredient isolated from the whole herb of Erigeron breviscapus (Vant.) Hand-Mazz, mainly scutellarin (also known as breviscapus, scutellarin, hereinafter referred to as B) , the chemical name is 4′5,6-trihydroxyflavone-7-O-glucuronide. The breviscapine raw material drug purchased from the market is analyzed by HPLC, and the content of B is about 90%. This preparation has been widely used clinically to treat cardiovascular and cerebrovascular diseases, and its curative effect is remarkable. However, its injection has poor stability and short storage time. Clinically, individual patients may experience cold and heat reactions, skin itching, and rashes after use. The appearance of the phenomenon is mainly ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07
Inventor 张人伟程惠佳樊献俄
Owner KUNMING LONGJIN PHARMA
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