Scutellarin raw material drug preparing method

A technology for scutellarin and raw materials, which is applied in the field of preparation of high-purity scutellarin, can solve the problems of low yield and the like, and achieves the effects of simple process steps and easy industrial production.

Inactive Publication Date: 2006-10-25
CHIATAI QINGCHUNBAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The deficiency of this method is that the yield is on the low side, and the purity can only reach more than 90% due to similar flavonoid structure molecules with scutellarin in methanol.

Method used

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  • Scutellarin raw material drug preparing method
  • Scutellarin raw material drug preparing method
  • Scutellarin raw material drug preparing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Weigh 1000g of commercially available breviscapine crude drug, add 30 times the weight of water, adjust the pH value to 7.8 with 10% potassium carbonate test solution, make it completely dissolved, filter, add ethanol precipitation with 1 times the amount of water to the filtrate, and stir while adding , to make the precipitation complete, let stand for 10 hours, filter, add ethanol to wash three times, then move the precipitate to another container, add 25 times the amount of water to dissolve, add 20 times the amount of ethanol, stir, filter, and add 1: 1 Hydrochloric acid to adjust the pH to 2-3 and let it stand for 10 hours, suction filter, wash with water until neutral, wash with ethanol once, dry, and repeat the above steps once. It is refined scutellarin, and its B content is 99.83% through HPLC analysis, as attached figure 1 shown.

Embodiment 2

[0037] Weigh 1000g of commercially available breviscapine crude drug, add 15 times the weight of water, adjust the pH value to 6.8 with 10% ammonium carbonate test solution, make it completely dissolved, filter, add 2 times the amount of water to the filtrate to precipitate methanol, and stir while adding , to make the precipitation complete, let stand for 10 hours, filter, add methanol to wash three times, then move the precipitate to another container, add 20 times the amount of water to dissolve, add 10 times the amount of methanol, stir, filter, and add 1: 1 hydrochloric acid to adjust the pH to 1-2 and let stand for 10 hours, filter with suction, wash with water until neutral, then wash with ethanol once, and dry to obtain refined scutellarin. The content of scutellarin is 98.97% by HPLC analysis, as shown in the attached figure 2 shown.

Embodiment 3

[0039] Weigh 1000g of commercially available scutellarin raw material, add 10 times the weight of water, adjust the pH value to 7.2 with 10% potassium bicarbonate test solution, dissolve completely, filter, add 1.5 times the amount of water to the filtrate to precipitate with acetone, and stir while adding , to make the precipitation complete, let stand for 10 hours, filter, add acetone to wash three times, then move the precipitate to another container, add 12 times the amount of water to dissolve, add 6 times the amount of acetone, stir, filter, and add 1: 1 hydrochloric acid to adjust the pH to 1-2 and let it stand for 10 hours, suction filter, wash with water until neutral, then wash with ethanol once, and dry to obtain refined scutellarin. The content of scutellarin is 99.13% by HPLC analysis, as shown in the attached image 3 shown.

Description of drawings

[0040] Instrument Type: High Performance Liquid Chromatography Gradient Mode: Constant Current

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Abstract

The invention relates to a manufacture method for high purity scutellarin bulk drug. It includes the following steps: adding scutellarin raw extractive into the container, adding water and adjusting the pH value to target value, whisking to fully dissolve; adding deposition solvent into the liquid, depositing, standing, filtering and washing by deposition solvent; transferring the deposition to suitable container, adding water for dissolving, adding solvent to make the liquid has a certain range of solvent ratio, whisking, filtering, adding acid to adjust the pH value to target value, depositing, washing to neutral, drying; repeating the previous steps for several times, the scutellarin with the content over 98% could be gained.

Description

technical field [0001] The invention relates to a method for preparing raw materials in the pharmaceutical industry, in particular to a method for preparing high-purity scutellarin. Background technique [0002] Scutellarin, also known as scutellarin, baicalein, scutellarin, scutellarin, and baicalin (from the Handbook of Active Ingredients in Plant Medicine: People's Medical Publishing House, March 1986, first edition, p946 ), the chemical name is 4′, 5, 6-trihydroxyflavone-7-0-glucuronide. Its structural formula is as follows: [0003] [0004] Scutellaria altissima L. leaves of labial plants, Scutellaria altissima L. leaves, stems and leaves of Scutellaria baicalensis Georgi, Erigeronbreviscapus (Vant.) Hand-Mazz and other plants of Compositae have a certain content of scutellarin . [0005] Erigeron breviscapus (Vant.) Hand-Mazz is a flavonoid active ingredient isolated from the whole herb of Erigeron breviscapus (Vant.) Hand-Mazz. It is a flavonoid active fraction...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07A61K31/7048A61P9/00
Inventor 黎豫杭张善飞潘迎锋刘晓云柴建国张建兵尤国鸿葛晶晶张丽张平
Owner CHIATAI QINGCHUNBAO PHARMA
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