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Method for detecting fasudil hydrochloride and related substances thereof

A technology for fasudil hydrochloride and related substances, applied in the field of medicine, can solve the problems of poor sensitivity, poor detection peak shape, inability to separate and detect isoquinoline and the like

Pending Publication Date: 2022-06-03
GRAND PHARM (CHINA) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the detection methods for fasudil hydrochloride and its related substances have disadvantages such as low resolution, poor sensitivity, and poor detection peak shape between related substances and main peaks and related substances. phylloline, isoquinoline-5-sulfonic acid, fasudil dimer, N,N-dimethylisoquinoline-5-sulfonamide, 8-position isomer of fasudil hydrochloride, isoquinoline- Related substances such as 8-sulfonic acid, N-oxide and N-hydroxyfasudil

Method used

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  • Method for detecting fasudil hydrochloride and related substances thereof
  • Method for detecting fasudil hydrochloride and related substances thereof
  • Method for detecting fasudil hydrochloride and related substances thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] In this embodiment, fasudil hydrochloride injection is detected according to the following method:

[0054] 1. Prepare the sample solution

[0055] Blank solution: water.

[0056] Mixed reference solution: Take about 10 mg of isoquinoline and place it in a 20 ml volumetric flask, dilute to the mark with methanol, shake well, and use it as the isoquinoline reference solution. Take 4 mg of impurity 15, fasudil dimer, impurity 10, impurity A, impurity B, impurity D, and impurity E respectively and place them in different 10ml volumes, add methanol to dilute to the mark, shake well, and serve as the control of each impurity product solution. Take 100 μl of the above 8 impurity reference substance solutions and place them in the same 10ml volumetric flask, add 4 mg of fasudil hydrochloride reference substance, dissolve in water and dilute to the mark, shake well, and use it as a mixed control solution. (See Table 1 for the names of impurities)

[0057] Table 1 Impurity n...

Embodiment 2

[0088] In this embodiment, the influence of different chromatographic columns on the detection of fasudil hydrochloride injection is studied, and the specific steps are as follows:

[0089] 1. Prepare the sample solution

[0090] Blank solution: water.

[0091] Oxidative destruction of the test solution: take 1.00ml of Fasudil hydrochloride injection and put it in a 50ml volumetric flask, add 1.0ml of 30% hydrogen peroxide, shake well, leave it for 30 minutes, dilute to the mark with water, and shake well. As the oxidative destruction of the test solution.

[0092] 2. Perform high-performance liquid chromatography detection on the blank solution and the oxidatively damaged test solution respectively. The detection conditions are as follows:

[0093] Chromatographic column: Welch Ultimate AQ-C18 150×4.6mm, 5μm or Welch Xtimate C18 250×4.6mm, 5μm;

[0094] Detection wavelength: 275nm;

[0095] Injection volume: 20μl;

[0096] Column temperature: 30℃;

[0097] Flow rate: 1....

Embodiment 3

[0103] In this embodiment, the influence of different elution conditions on the detection of fasudil hydrochloride injection is studied, and the specific steps are as follows:

[0104] 1. Prepare the sample solution

[0105] Blank solution: water.

[0106] Mixed reference solution: take about 10 mg of isoquinoline and place it in a 20 ml volumetric flask, dilute to the mark with methanol, shake well, and use it as the isoquinoline reference solution. Take 4 mg of impurity 15, fasudil dimer, impurity 10, impurity A, impurity B, impurity D, and impurity E respectively and place them in different 10ml volumes, add methanol to dilute to the mark, shake well, and serve as the control of each impurity product solution. Take 100 μl of the above 8 impurity reference substance solutions and put them in the same 10ml volumetric flask, add 4 mg of fasudil hydrochloride reference substance, dissolve in water and dilute to the mark, shake well, and use it as a mixed control solution. (S...

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Abstract

The invention provides a method for detecting fasudil hydrochloride, which comprises the following steps: a fasudil hydrochloride sample is subjected to high performance liquid chromatography detection, the mobile phase adopted by the high performance liquid chromatography detection comprises a mobile phase A and a mobile phase B, the pH value of the mobile phase is 3.0-4.0, the mobile phase A is selected from an ammonium dihydrogen phosphate solution, the mobile phase B is selected from an ammonium dihydrogen phosphate solution, and the mobile phase C is selected from an ammonium dihydrogen phosphate solution. The mobile phase B is selected from methanol. The method for detecting fasudil hydrochloride can effectively separate and detect fasudil hydrochloride and related substances thereof, has the advantages of high accuracy, high separation degree, low detection limit, high stability, simplicity and convenience in operation, rapidness, high efficiency and the like, and is suitable for wide application.

Description

technical field [0001] The present invention relates to the field of medicine. Specifically, the present invention relates to a detection method for fasudil hydrochloride and related substances thereof. Background technique [0002] Fasudil hydrochloride is a new type of drug with a wide range of pharmacological effects. Its molecular structure is shown in the following formula. It is an RHO kinase inhibitor. It dilates blood vessels by increasing the activity of myosin light chain phosphatase and reduces the tension of endothelial cells. , improve the microcirculation of brain tissue, do not produce and aggravate the stealing of blood in the brain, at the same time can antagonize inflammatory factors, protect nerves against apoptosis, and promote nerve regeneration. [0003] [0004] Relevant substances are mainly starting materials, intermediates, polymers, side reaction products, degradation products during storage, etc. brought in during the production process. Rese...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 钟怡朱婷谢秀苹王芝秦巨波詹志斌
Owner GRAND PHARM (CHINA) CO LTD
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