Method for detecting fasudil hydrochloride and nine related substances of fasudil hydrochloride

Abstract

The invention provides a method for detecting fasudil hydrochloride and nine related substances of the fasudil hydrochloride. The method comprises the following steps that a system suitability solution, a test solution and a reference solution are prepared, the solutions are injected into a high performance liquid chromatograph for detection, and the content of fasudil hydrochloride and the related substances of fasudil hydrochloride is calculated according to an external standard method; the method is characterized in that the detection conditions comprises the following conditions that a chromatographic column is an alkyl bonded silica gel packed column; a detector is a diode array detector; the detection wavelength is 240-290nm; the column temperature is 20-35 DEG C; the injection volume is 10-100[mu]l; the flow rate is 0.5-2.0ml/min; a mobile phase is buffer salt-organic phase, and pH of the buffer salt is adjusted to 3-5; and a elution method is gradient elution. The method has the following technical effects that the detection method can detect fasudil hydrochloride and nine related substances, the separation degree between fasudil hydrochloride and the related substances meets the requirements (greater than 2.0), and the number of theoretical plates is high and the tailing factor is good.

Description

technical field [0001] The invention belongs to the field of drug analysis, and relates to an analysis and detection of a drug, in particular to a high-performance liquid chromatography, which utilizes characteristic peak absorption to quantitatively detect fasudil hydrochloride and nine related substances. Background technique [0002] Fasudil hydrochloride, chemical name hexahydro-1-(5-isoquinolinesulfonyl)-1H-1,4 diazepine hydrochloride, is a RHO kinase inhibitor, which can be used to improve and prevent Cerebral vasospasm and subsequent cerebral ischemic symptoms after subarachnoid hemorrhage. [0003] In the clinical application of Fasudil hydrochloride, sometimes elevated alanine aminotransferase and aspartate aminotransferase, rash, dysuria or polyuria, vomiting, headache and other adverse reactions may occur, which may be related to the impurities. [0004] After searching, the Chinese patent application CN201810429938.3, the patent name is HPLC detection method for...

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Problems solved by technology

[0004] After searching, the Chinese patent application CN201810429938.3, the patent name is HPLC detection method for related substances of fasudil hydrochloride, provides a kind of related impurities of fasudil hydrochloride 5-isoquinolinesulfonic acid, pyridine N-oxyfasudil The method for the determination of dil, 1-hydroxyfasudil, 8-quinoline fasudil, 8-position isomer, piperazine condensate, N-hydroxyfasudil and dimer, but its There are also certain technical problems: when this method detects Fasudil hydrochloride, impurity F (i.e. the 6-position isomer), and impurity G (i.e. the 8-position isomer), the degree of separation cannot meet the requirements and cannot be accurate. Measure the content of these three substances

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