A kind of preparation method of breviscapine crude drug

A technology for breviscapine and raw materials, which is applied in the field of preparation of high-purity breviscapine raw materials, and achieves the effects of simple preparation process, overcoming solvent residues, and easy industrial production.

Inactive Publication Date: 2014-10-08
红河健生源生物技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the conventional preparation method of high-content scutellarin API requires the use of resin and a large amount of acetone solvent, the residual substances in the product are difficult to control, and the process is complicated, the production cost is high, and it is easy to cause pollution to the human body and the environment

Method used

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  • A kind of preparation method of breviscapine crude drug
  • A kind of preparation method of breviscapine crude drug
  • A kind of preparation method of breviscapine crude drug

Examples

Experimental program
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Effect test

Embodiment 1

[0020] The raw material of scutellaria breviscapine was extracted with ethanol to obtain crude scutellarin, and the content of scutellarin was detected to be 80.8%. figure 1 For its high-performance liquid chromatography, the detection method and chromatographic conditions are all carried out according to the regulations of the 2010 edition of "Chinese Pharmacopoeia". Weigh 1000g of crude scutellarin, add 35°C warm water to prepare a feed solution with a concentration of 10% by weight, and use 10% NaHCO 3 Adjust the pH to 6.7-7.0, dissolve and filter, centrifuge the filtrate with a 16000r / min continuous tube centrifuge, and then perform fine filtration, adjust the concentration of the filtrate to 10%, heat the temperature to 50°C, adjust the pH to 6.7-7.0, and pack the filtrate Put it into the crystallization tank and let it stand, the total time for natural cooling and crystallization is 60 hours; it takes 38 hours for the temperature of the feed liquid to drop from 50°C to ...

Embodiment 2

[0022] Take by weighing 1000g of the breviscapine raw material product obtained in Example 1, prepare it into a concentration of 6% by weight, and use 10% NaHCO 3 Adjust the pH to 7.0 to dissolve completely, add activated carbon for needles with a product weight ratio of 3%, heat to 60°C and stir for half an hour to filter while hot, the resulting liquid is clear and transparent, take the filtrate to adjust the concentration to 6.0%, and heat to 80-82 ℃, after adjusting the pH to 6.7-7.0, set the crystallization tank to stand still for 60 hours to crystallize, and cool and crystallize for 48 hours in two stages. The temperature of the filtrate is dropped from 60°C to 46°C. Higher than 0.5°C; the second stage is from 45°C to 22°C, which takes a total of 20 hours, the temperature drop is not higher than 1.15°C per hour, and the crystal is grown for 12 hours; The temperature drops to 22°C, the rotation speed in the tank is 3min / 360°, the crystallization tank and the discharge sys...

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Abstract

The invention discloses a preparation method of a high-purity scutellarin crude drug. The crude product of scutellarin is first made into a crystal solution, and the crystals are obtained after standing still, and then the crystals are dissolved, precipitated, filtered, dehydrated, and dried to obtain a scutellarin product with a content of more than 90%. After further purification, a scutellarin product with a content of more than 98% is obtained. The preparation process of the invention is simple, easy for industrial production, and solves the difficult problem of refining scutellarin raw material medicine for many years. Because the crystallization method makes the same molecules orderly arranged, only the same crystal lattice molecules can crystallize and precipitate, and other substances are different from each other due to different crystal lattices. Separation of scutellarin effectively overcomes the problem of solvent residues, and removes other impurities at the same time, and the prepared scutellarin raw material meets the standards stipulated in the 2010 edition of "Chinese Pharmacopoeia".

Description

technical field [0001] The invention belongs to the technical field of herbal medicine production, and in particular relates to a preparation method of a high-purity scutellarin bulk medicine. Background technique [0002] Erigeron breviscapus (Vant.) Hand.Mazz., also known as Erigeron breviscapus, belongs to the genus Erigeron breviscapus (Vant.) Hand. Erigeron breviscapus is cultivated through artificial domestication. In 2009, Erigeron breviscapus was approved as a national geographical indication protection product. At present, the conventional preparation method of high-content scutellarin bulk drug requires the use of resin and a large amount of acetone solvent, the residual substances in the product are difficult to control, and the process is complicated, the production cost is high, and it is easy to cause pollution to the human body and the environment. Contents of the invention [0003] The purpose of the present invention is to address the deficiencies of t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/07C07H1/08
Inventor 杨建文倪建芳王升云吴道聪
Owner 红河健生源生物技术有限公司
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