Detection analysis method for impurity homopiperazine in fasudil hydrochloride

The technology of an analysis method of fasudil hydrochloride is applied in the field of detection and analysis of the impurity homopiperazine in fasudil hydrochloride, which can solve the problems that the quality of the product is difficult to control and is not suitable for gas phase detection, etc., and achieves high accuracy, The effect of small harm and simple operation

Active Publication Date: 2014-07-02
JIANGSU WANBANG BIOPHARMLS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Homopiperazine is used as the starting material for the synthesis of fasudil hydrochloride. Product quality control considers that it will have residues. Combined with production process analysis, homopiperazine will generate homopiperazine hydrochloride during the reaction process. Oxyzine has no ultraviolet absorption, and it is not suitable for gas phase detection after salt formation, so it is difficult to control the quality of products in production

Method used

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  • Detection analysis method for impurity homopiperazine in fasudil hydrochloride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Determination according to ion chromatography (Chinese Pharmacopoeia 2010 edition two appendix Ⅴ J).

[0038] Chromatographic conditions and system suitability test Use carboxylic acid group-bonded silica gel as filler; 5mmol / L methanesulfonic acid aqueous solution-acetonitrile (90:10) as mobile phase; flow rate 1.0ml per minute; conductometric detection. Weigh each appropriate amount of fasudil hydrochloride and homopiperazine reference substance, dissolve and dilute with mobile phase to make a mixed solution containing about 3 mg of fasudil hydrochloride and 3 μg of homopiperazine in every 1 ml as the system suitability test solution, Precisely measure 20 μl and inject it into the liquid chromatograph, record the chromatogram, and the separation degree between the homopiperazine peak and the adjacent peak should meet the requirements.

[0039] Determination method Take about 0.3g of this product, weigh it accurately, put it in a 100ml measuring bottle, add mobile phas...

Embodiment 2

[0041] Determination according to ion chromatography (Chinese Pharmacopoeia 2010 edition two appendix Ⅴ J).

[0042] Chromatographic conditions and system suitability test Use carboxylic acid group-bonded silica gel as filler; 5mmol / L methanesulfonic acid aqueous solution-acetonitrile (75:25) as mobile phase; flow rate 0.3ml per minute; conductometric detection. Weigh each appropriate amount of fasudil hydrochloride and homopiperazine reference substance, dissolve and dilute with mobile phase to make a mixed solution containing about 3 mg of fasudil hydrochloride and 3 μg of homopiperazine in every 1 ml as the system suitability test solution, Precisely measure 20 μl and inject it into the liquid chromatograph, record the chromatogram, and the separation degree between the homopiperazine peak and the adjacent peak should meet the requirements.

[0043] Determination method Take about 0.3g of this product, weigh it accurately, put it in a 100ml measuring bottle, add mobile phas...

Embodiment 3

[0045] Determination according to ion chromatography (Chinese Pharmacopoeia 2010 edition two appendix Ⅴ J).

[0046] Chromatographic conditions and system suitability test Use carboxylic acid group bonded silica gel as filler; use 5mmol / L methanesulfonic acid aqueous solution-acetonitrile (95:5) as mobile phase; flow rate is 2ml per minute; conductivity detection. Weigh each appropriate amount of fasudil hydrochloride and homopiperazine reference substance, dissolve and dilute with mobile phase to make a mixed solution containing about 3 mg of fasudil hydrochloride and 3 μg of homopiperazine in every 1 ml as the system suitability test solution, Precisely measure 20 μl and inject it into the liquid chromatograph, record the chromatogram, and the separation degree between the homopiperazine peak and the adjacent peak should meet the requirements.

[0047]Determination method Take about 0.3g of this product, weigh it accurately, put it in a 100ml measuring bottle, add mobile pha...

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Abstract

The invention discloses a detection analysis method for impurity homopiperazine in fasudil hydrochloride, wherein conductivity detection and an ion chromatography method are adopted to carry out quantitative analysis on the impurity homopiperazine in fasudil hydrochloride. The method has characteristics of simpleness, high precision, good stability, and good reproducibility.

Description

[0001] technical field [0002] The invention relates to a method for detecting and analyzing fine chemical products, in particular to a method for detecting and analyzing impurity homopiperazine in fasudil hydrochloride. Background technique [0003] Fasudil hydrochloride is a new type of drug with a wide range of pharmacological effects. Its molecular structure is a 5-isoquinoline sulfonamide derivative, which is an RHO kinase inhibitor and expands blood vessels by increasing the activity of myosin light chain phosphatase , reduce the tension of endothelial cells, improve the microcirculation of brain tissue, prevent and aggravate cerebral blood stealing, and at the same time antagonize inflammatory factors, protect nerves against apoptosis, and promote nerve regeneration. The results show that fasudil hydrochloride has a certain effect on promoting the recovery of nerve function, relieving clinical symptoms and reducing the disability rate. Therefore, due to the cons...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 王成刘跃跃张山乔德水高雪芹
Owner JIANGSU WANBANG BIOPHARMLS
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