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Method for determination of content of related impurity (5-methyl isoquinolinesulfonic acid) of fasudil hydrochloride

A technology of methyl isoquinolinesulfonate and fasudil hydrochloride, which is applied in the field of high-performance liquid chromatography analysis and detection of fasudil hydrochloride impurity 5-isoquinolinesulfonate methyl ester, can solve the problem of 5-isoquinolinesulfonate Solvent problems such as weak absorption, non-detection, and poor separation effect of methyl phenol sulfonate, to achieve the effects of good stability and reproducibility, high sensitivity, high accuracy and precision

Inactive Publication Date: 2018-08-14
SHANDONG XINHUA PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] (1) Under this condition, the separation effect of methyl 5-isoquinolinesulfonate and fasudil hydrochloride is poor, and the chromatographic peaks basically overlap together, and the baseline separation cannot be achieved;
[0012] (2) Under this condition, the absorption of methyl 5-isoquinolinesulfonate is extremely weak and cannot be detected

Method used

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  • Method for determination of content of related impurity (5-methyl isoquinolinesulfonic acid) of fasudil hydrochloride
  • Method for determination of content of related impurity (5-methyl isoquinolinesulfonic acid) of fasudil hydrochloride
  • Method for determination of content of related impurity (5-methyl isoquinolinesulfonic acid) of fasudil hydrochloride

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Experimental program
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Effect test

Embodiment 1

[0031] Experimental Equipment and Reagents

[0032] (1) Experimental equipment:

[0033] Instrument: Shimadzu 20A with UV detector

[0034] (2) Chromatographic conditions:

[0035] Chromatographic column: ACCHROM XAmide column, 4.6×250mm, 5um;

[0036] Flow rate: 0.9~1.1ml / min;

[0037] The detection wavelength is 238nm;

[0038] Column temperature: 28~32℃;

[0039] Injection volume: 20ul;

[0040] mobile phase:

[0041] A: 0.05mol / l ammonium dihydrogen phosphate aqueous solution;

[0042] B: Methanol;

[0043] A:B=(91~94):(6~9)(V:V)

[0044] (3) Experimental reagents:

[0045] Methanol: Beijing Bailingwei Technology Co., Ltd., HPLC grade;

[0046] Ammonium dihydrogen phosphate: Sinopharm chemical reagent, analytical grade

[0047] Implementation steps:

[0048] 1. Precisely measure 20 μl of the mobile phase, inject it into the liquid chromatograph, and record the chromatogram; the result has no interference with the determination of impurities. Accurately weigh ...

Embodiment 2

[0051] Experimental Equipment and Reagents

[0052] (1) Experimental equipment:

[0053] Instrument: Shimadzu 20A with UV detector

[0054] (2) Chromatographic conditions:

[0055] Chromatographic column: ACCHROM XAmide column, 4.6×250mm, 5um;

[0056] Flow rate: 1.0ml / min;

[0057] The detection wavelength is 238nm;

[0058] Column temperature: 30°C;

[0059] Injection volume: 20ul;

[0060] Mobile phase: 0.05mol / l ammonium dihydrogen phosphate aqueous solution:methanol=92:8(V:V)

[0061] (3) Experimental reagents:

[0062] Methanol: Beijing Bailingwei Technology Co., Ltd., HPLC grade;

[0063] Ammonium dihydrogen phosphate: Sinopharm chemical reagent, analytical grade

[0064] Implementation steps:

[0065] Take about 250mg of Fasudil hydrochloride, weigh it accurately, put it in a 25ml measuring bottle, add 20ml of methanol to dissolve, then accurately add 1.0ml of impurity standard stock solution, dilute to the mark with methanol, shake well, and use it as a precis...

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Abstract

The invention provides a method for determination of the content of a related impurity (5-methyl isoquinolinesulfonic acid) of fasudil hydrochloride. The method is characterized in that a reversed-phase high-performance liquid chromatographic peak area normalization method is adopted for quantitative analysis; for the chromatographic conditions, the chromatographic column is an ACCHROM XAmide column; the flow speed is 0.9-1.1ml / min; the detection wavelength is 238nm; the column temperature is 28-32 DEG C; the sample injection amount is 20mu l; a mobile phase A is 0.05mol / l ammonium dihydrogenphosphate aqueous solution; a mobile phase B is methanol; A:B is equal to (91-94): (6-9) (V:V). The method provided by the invention is convenient to control the product quality in the processes of production and quality control, and has the advantages of low cost, simpleness, easy implementation, high accuracy and precision, good stability and reproducibility and high sensitivity.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and in particular relates to a high-performance liquid chromatography analysis and detection method for fasudil hydrochloride impurity 5-isoquinolinesulfonate methyl ester. Background technique [0002] Fasudil Hydrochloride (Fasudil Hydrochloride), its chemical name is hexahydro-1-(5-isoquinolinesulfonyl)-1H-1,4-diazepine hydrochloride, molecular formula: C 14 h 17 N 3 o 2 S·HCL, molecular weight: 327.83. [0003] Its structural formula is: [0004] [0005] Fasudil is a RHO kinase inhibitor and intracellular Ca 2+ Antagonist, its mode of action is to dilate 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 brain blood steal, and at the same time antagonize inflammatory factors and protect Nerve anti-apoptosis, promote nerve regeneration. Clinical...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 丰宇胜郑忠辉徐豪杰王剑平李丹
Owner SHANDONG XINHUA PHARMA CO LTD
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