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Preparation process of high-purity scutellarin bulk drug

A technology for breviscapine and preparation technology, which is applied in the field of preparation technology of high-purity raw materials, can solve problems such as incomplete removal, and achieve the effects of easy separation and convenient automatic control.

Active Publication Date: 2011-11-30
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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  • Preparation process of high-purity scutellarin bulk drug
  • Preparation process of 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. The purity of B as determined by HPLC 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 preparation process of high-purity crude drug in pharmacy. The process of the present invention consists of the following steps: 1. Add water 2-15 times the weight of the crude product to the crude product of scutellarin, stir, and then add arginine, lysine or hydroxylysine with a weight of 35-55% of the crude product Acid, heating, the temperature is 45 ℃ to boiling, make a stable aqueous solution, filter, remove the filter residue; 2. Add acid phosphate 0.1-2.0 times the weight of the crude scutellarin to the filtrate while it is hot, and the acid phosphate is prepared as a weight percentage 10-30% aqueous solution; then add an organic solvent 2-3 times the volume of the combined solution to crystallize scutellarin; 3. add water more than 10 times the weight of the crude product of scutellarin to the crystallization, Boil, and after the solution is cooled to below 60°C, add an organic acid conversion agent 0.2-1.0 times the weight of crude scutellarin to reduce scutellarin salt to scutellarin, filter and dry the precipitate to obtain High-purity scutellarin raw material.

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 Patents(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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