Process for preparing high-purity scutellarin bulk drug

A preparation technology of scutellarin, which is applied in the field of preparation technology of high-purity raw materials, can solve problems such as incomplete elimination, and achieve the effect of easy separation and automatic control

Active Publication Date: 2010-06-16
KUNMING LONGJIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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.

Method used

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  • Process for preparing high-purity scutellarin bulk drug
  • Process for preparing high-purity scutellarin bulk drug

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: Weigh 10kg of crude raw material with scutellarin content of 89.25%, add 50L of water and stir, add 38L of 10% arginine solution and heat to boiling, add water to make 100L aqueous solution, filter out insoluble matter, and filtrate while hot Add 50L of 10% sodium dihydrogen phosphate solution while stirring, then add 450L of acetone while stirring to make scutellarin crystallize, after standing for 3 hours, filter, drain the acetone, add 150L of water to boil and discard Remaining organic solvent, when the solution is cooled to below 60°C, add 25L of 20% glacial acetic acid solution, let it stand for 2 hours, filter it with suction, and dry it to obtain 6.25kg of dry product; it is the raw material of high-purity scutellarin. As determined by HPLC, the purity of B is 99.5907%, such as figure 1 shown.

Embodiment 2

[0027] Example 2: Weigh 20kg of crude raw material with scutellarin content of 84.24%, add 100L of water and stir, add 38L of 20% arginine solution and heat to boiling, add water to make 200L aqueous solution, filter out insoluble matter, and put the model on the filtrate It is AB-8 macroporous resin column chromatography. After discarding the pigment and macromolecular substances, collect the eluate and concentrate it to about 200L by distillation. Add 100L of 10% potassium dihydrogen phosphate solution while stirring the concentrated solution while it is hot. Then add 800L of acetone while stirring to crystallize scutellarin. After standing for 3 hours, filter, drain the acetone, add 200L of water to boil and discard the residual organic solvent. When the solution is cooled to below 60°C, add 50L of 20% acetic anhydride solution was left to stand for 2 hours, suction filtered, and dried to obtain 11.61kg of dry product, which was the raw material of high-purity scutellarin. T...

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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 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08
Inventor 张人伟赵尔跃樊献俄
Owner KUNMING LONGJIN PHARMA
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