A method for detecting fasudil hydrochloride and its nine related substances

Abstract

The invention provides a method for detecting fasudil hydrochloride and nine related substances thereof, comprising the following steps: preparing a system applicability solution, a test solution and a reference solution, and injecting the above solutions into a high performance liquid chromatograph Detect, calculate the content of fasudil hydrochloride and its related substances by the external standard method; It is characterized in that, detection condition is as follows: chromatographic column is an alkyl bonded silica gel packed column; Detector is a diode array detector; Detection wavelength 240~ 290nm; column temperature 20~35℃; injection volume 10~100μl; flow rate 0.5~2.0ml / min; mobile phase is buffer salt-organic phase, buffer salt adjusts pH to 3-5; elution method is gradient elution. The present invention has the following technical effects: the detection method of the present invention can detect fasudil hydrochloride and nine related substances, and the separation degree between fasudil hydrochloride and related substances all meets the requirements (greater than 2.0), and the theoretical plate The higher the number, the better the tailing factor.

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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