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HPLC detection method for fasudil hydrochloride related substances

A technology for fasudil hydrochloride and related substances, applied in the field of drug analysis, can solve problems such as poor buffering capacity, achieve the effects of high accuracy and precision, good stability and reproducibility, and facilitate the control of product quality

Active Publication Date: 2018-09-28
SHANDONG XINHUA PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] (2) Mobile phase triethylamine aqueous solution-methanol system has poor buffering capacity

Method used

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  • HPLC detection method for fasudil hydrochloride related substances
  • HPLC detection method for fasudil hydrochloride related substances
  • HPLC detection method for fasudil hydrochloride related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Experimental Equipment and Reagents

[0047] (1) Experimental equipment:

[0048] Instrument: Shimadzu liquid chromatograph LC-20AT with UV detector

[0049] (2) Chromatographic conditions:

[0050] Column: Phenomenex 5μm C18 250×4.6mm

[0051] Flow rate: 1.0ml / min;

[0052] Detection wavelength: 275nm;

[0053] Column temperature: 30°C;

[0054] Injection volume: 20μl

[0055] Mobile phase A: Phosphate buffer (pH7.0) (take 5.44g of potassium dihydrogen phosphate and 0.65g of sodium hydroxide, add water to dissolve and dilute to 2000ml, adjust the pH value to 7.0 with 2mol / L sodium hydroxide solution)- Methanol (85:15),

[0056] Mobile phase B: Phosphate buffer (pH7.0)-methanol (40:60). Carry out gradient elution according to the following table:

[0057] Table 1 Gradient elution program

[0058]

[0059] (3) Experimental reagents:

[0060] Methanol: Beijing Bailingwei Technology Co., Ltd., HPLC grade;

[0061] Sodium hydroxide: Sinopharm chemical rea...

Embodiment 2

[0070] Experimental Equipment and Reagents

[0071] (1) Experimental equipment:

[0072] Instrument: Shimadzu liquid chromatograph LC-20AT with UV detector

[0073] (2) Chromatographic conditions:

[0074] Column: different batches of Phenomenex 5μm C18 250×4.6mm

[0075] Flow rate: 0.9~1.1ml / min;

[0076] Detection wavelength: 275nm;

[0077] Column temperature: 28~32℃;

[0078] Injection volume: 20μl

[0079] Mobile phase A: Phosphate buffer (pH6.95~7.05) (take 5.44g of potassium dihydrogen phosphate and 0.65g of sodium hydroxide, add water to dissolve and dilute to 2000ml, adjust the pH value to 6.95 with 2mol / L sodium hydroxide solution ~7.05)-methanol (85:15),

[0080] Mobile phase B: Phosphate buffer (pH6.95~7.05)-methanol (40:60). Carry out gradient elution according to the following table:

[0081] Table 1 Gradient elution program

[0082]

[0083] (3) Experimental reagents:

[0084] Methanol: Beijing Bailingwei Technology Co., Ltd., HPLC grade;

[0...

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Abstract

The invention provides a content determination method for fasudil hydrochloride related impurities, namely 5-isoquinoline sulfonic acid, pyridine N-oxyfasudil, 1-hydroxyfasudil, 8-quinoline fasudil, an 8-isomer, a piperazine condensation compound, N-hydroxyfasudil and a dimer. Quantitative analysis is performed by a reversed-phase high performance liquid chromatography peak area normalization method, and a chromatographic column with an octadecyl bonded phase as a stationary phase is used; the detection wavelength is 275nm; a mobile phase A is a phosphate buffer (pH of 6.95-7.05)-methanol (85:15), a mobile phase B is a phosphate buffer (pH of 6.95-7.05)-methanol (40:60), and gradient elution is performed. By the content determination method, product quality control during production and quality control is facilitated; the content determination method has the advantages of low cost, simplicity, easiness in implementation, high accuracy and precision and good stability and reproducibility.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and in particular relates to an HPLC detection method for fasudil hydrochloride related substances. Background technique [0002] Fasudil Hydrochloride (Fasudil Hydrochloride), its chemical name is hexahydro-1-(5-isoquinolinesulfonyl)-1(H)-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. Clinically, it can be used to prevent and improve vasospasm after subarachnoid ...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 王付荣郑忠辉徐豪杰王剑平李丹
Owner SHANDONG XINHUA PHARMA CO LTD
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