Process for preparing high-purity scutellarin bulk drug

Abstract

The invention relates to a process for preparing a high-purity bulk drug in pharmaceutics. The process comprises the following steps: (1) adding water with the weight 2-15 times of the weight of a crude product into the breviscapine crude product, stirring, then adding arginine, lysine or hydroxylysine with the weight 35-55% of the weight of the crude product, heating at the temperature of 45 DEG C until boiling off to prepare a stable water solution, filtering and removing the discarded filter residue; (2) adding acid phosphate with the weight 0.1-2.0 times of the weight of the breviscapine crude product into the hot filtrate and preparing the acid phosphate into a water solution with the weight percent of 10-30%; then adding an organic solvent with the volume 2-3 times of the volume of merging liquid and crystallizing scutellarin; and (3) adding the water with the weight more than 10 times of the weight of the breviscapine crude product into the crystal, boiling off, then adding a transforming agent of organic acid with the weight 0.2-1.0 time of the weight of the breviscapine crude product after cooling the solution to the temperature below 60 DEG C and reducing scutellarin salt into the scutellarin so as to obtain the high-purity scutellarin raw material after filtering a precipitate and drying.

Description

technical field [0001] The invention relates to a preparation process of a high-purity bulk drug in pharmacy, in particular to a large-scale, continuous and automatic preparation process of the bulk drug. Background technique [0002] Breviscapine is an active ingredient of flavonoids isolated from the whole herb of Erigeron breviscapus, also known as Erigeron breviscapus, the main ingredient of which is scutellarin, also known as scutellarin, chemical name: 4′5 , 6-trihydroxyflavone-7-0-glucuronide, molecular formula: C 21 h 18 o 12 , molecular weight: 462.37. Scutellarin belongs to flavonoid glycosides and is insoluble in water. Because it contains carboxyl groups, it can form salts with alkali or alkaline salts, and is easily soluble in water. Discard the water-insoluble matter. People take advantage of this property. Since 1984, a number of pharmaceutical companies have successively produced water injections and put them on the market. Due to the different processes ...

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Problems solved by technology

People take advantage of this property. Since 1984, many pharmaceutical factories have successively made water injections and put them on the market. Due to the different processes of each company, the HPLC analysis of the raw material of scutellarin shows that the content of B is between 75% and 90%. During the period, various preparations derived from it have been widely used in clinical treatment of cardiovascular and cerebrovascular diseases, and the curative effect is remarkable, but many adverse reactions have also occurred clinically, such as cold and hot reactions, skin itching, rash and other allergic phenomena. The occurrence of breviscapine is mainly due to the failure to remove some of the allergenic impurities in the production process of the API. This problem has not been resolved since the advent of breviscapine products for more than 30 years, and it was not gradually resolved until 2004.

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