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Preparation method of phenylephrine hydrochloride impurity standard substance

A technology of phenylephrine hydrochloride and standard product, which is applied in the preparation of organic compounds, chemical instruments and methods, preparation of aminohydroxy compounds, etc. Unable to meet the requirements of drug impurities, etc., to achieve the effect of high product yield and purity, and improve product purity

Active Publication Date: 2020-09-01
珠海安哲生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purity of norfeline hydrochloride obtained by the method disclosed in this patent is low, which cannot meet the requirements of pharmaceutical impurity standards, and the overall yield is also low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] A kind of preparation method of phenylephrine hydrochloride impurity standard substance, concrete steps are as follows:

[0040] (1) First place the phenylephrine hydrochloride bulk drug under light conditions to make it produce impurities, and then use preparative chromatography to obtain chromatographically pure target impurities through two preparations;

[0041] (2) Then, in the presence of ketoreductase KRED and reduced coenzyme II NADPH, react with nitromethane and m-hydroxybenzaldehyde as raw materials to obtain a light yellow oil, and then the light yellow oil is subjected to catalytic hydrogenation reaction, Filtration and concentration to obtain a concentrate;

[0042] (3) Then add the concentrate to the mixed solution of isopropanol-n-propyl acetate-acetonitrile with a volume ratio of 1:0.5:0.1, heat and stir to dissolve, then add the chromatographically pure target impurities neutralized by alkali, stand for crystallization, and filter , dry under reduced p...

Embodiment 2

[0064] A kind of preparation method of phenylephrine hydrochloride impurity standard substance, concrete steps are as follows:

[0065] (1) First place the phenylephrine hydrochloride bulk drug under light conditions to make it produce impurities, and then use preparative chromatography to obtain chromatographically pure target impurities through two preparations;

[0066] (2) Then, in the presence of ketoreductase KRED and reduced coenzyme II NADPH, react with nitromethane and m-hydroxybenzaldehyde as raw materials to obtain a light yellow oil, and then the light yellow oil is subjected to catalytic hydrogenation reaction, Filtration and concentration to obtain a concentrate;

[0067] (3) Add the concentrate to the mixed solution of isopropanol-n-propyl acetate-acetonitrile with a volume ratio of 1: 0.6:0.08, heat and stir to dissolve, then add the chromatographically pure target impurities neutralized by alkali, stand for crystallization, and filter , dry under reduced pres...

Embodiment 3

[0088] A kind of preparation method of phenylephrine hydrochloride impurity standard substance, concrete steps are as follows:

[0089] (1) First place the phenylephrine hydrochloride bulk drug under light conditions to make it produce impurities, and then use preparative chromatography to obtain chromatographically pure target impurities through two preparations;

[0090] (2) Then, in the presence of ketoreductase KRED and reduced coenzyme II NADPH, react with nitromethane and m-hydroxybenzaldehyde as raw materials to obtain a light yellow oil, and then the light yellow oil is subjected to catalytic hydrogenation reaction, Filtration and concentration to obtain a concentrate;

[0091] (3) Add the concentrate to the mixed solution of isopropanol-n-propyl acetate-acetonitrile with a volume ratio of 1:0.55:0.09, heat and stir to dissolve, then add the chromatographically pure target impurities neutralized by alkali, stand for crystallization, and filter , dry under reduced pres...

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PUM

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Abstract

The invention provides a preparation method of a phenylephrine hydrochloride impurity standard substance, which comprises the following steps: putting an phenylephrine hydrochloride bulk drug under anillumination condition to generate impurities, and obtaining chromatographically pure target impurities by preparative chromatography; in the presence of ketoreductase KRED and reduced coenzyme II NADPH, taking nitromethane and m-hydroxybenzaldehyde as raw materials to react to obtain a concentrate; and finally, recrystallizing the concentrate by using an isopropanol-n-propyl acetate-acetonitrilemixed solution, adding chromatographically pure target impurities neutralized by alkali in the recrystallization process, and salifying to obtain the phenylephrine hydrochloride impurity standard substance (impurity A) which is high in product yield and purity and meets the requirements of drug impurity standard substances.

Description

technical field [0001] The invention relates to the technical field of pharmacy, in particular to a preparation method of a phenylephrine hydrochloride impurity standard. Background technique [0002] Phenylephrine hydrochloride is used to prevent and treat hypotension caused by spinal anesthesia, general anesthesia, application of chlorpromazine, etc. It is also used for supraventricular tachycardia and mydriasis examination. Phenylephrine hydrochloride is an α-adrenergic receptor agonist, a sympathomimetic amine drug that acts directly on the receptor, but sometimes also works indirectly by promoting the release of phenylephrine from the storage site. Oxynephrine is similar, but weaker, longer lasting, and less toxic. It is usually used clinically in the aspects of infectious toxicity, anaphylactic shock, supraventricular acceleration, etc. It has good efficacy and safety, and has a very good clinical application prospect. The structural formula of phenylephrine hydrochl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/10C07C213/08C07C215/58
CPCC07C213/10C07C213/08C07C215/58
Inventor 蔡锦镇
Owner 珠海安哲生物科技有限公司
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