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A kind of detection method of methyl 5-isoquinolinesulfonate in fasudil hydrochloride

A technology of methyl isoquinolinesulfonate and fasudil hydrochloride is applied in the field of detection of methyl 5-isoquinolinesulfonate in fasudil hydrochloride, which can solve the problem of ineffective detection, insufficient sensitivity, and inability to detect problems such as problems, to achieve the effect of safety control, high detection sensitivity, and short running time

Active Publication Date: 2020-11-03
KPC PHARM INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (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;
[0006] (2) Under this condition, the absorption of methyl 5-isoquinolinesulfonate is extremely weak and cannot be detected
The quantitative concentration of this method is 0.337 μg / ml, and the detection limit concentration is 0.084 μg / ml, which is still high, and the sensitivity is not enough, and it cannot effectively detect methyl 5-isoquinolinesulfonate at the ppm level in fasudil hydrochloride

Method used

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  • A kind of detection method of methyl 5-isoquinolinesulfonate in fasudil hydrochloride
  • A kind of detection method of methyl 5-isoquinolinesulfonate in fasudil hydrochloride
  • A kind of detection method of methyl 5-isoquinolinesulfonate in fasudil hydrochloride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 1. Instruments and materials

[0045] 1. Main instruments

[0046] Mass spectrometer: ThermoScientific, Q Exactive TM Combined quadrupole Orbitrap mass spectrometer.

[0047] Liquid chromatograph: ThermoScientific Company, UltiMate3000 type.

[0048] Electronic balance: METTLER company, XP205 type.

[0049] 2. Experimental materials

[0050] Acetonitrile: Fisher Scientific, LC-MS grade.

[0051] 5-isoquinolinesulfonate methyl ester reference substance: provided by Kunming Pharmaceutical Group Co., Ltd., with a purity of 100.00%.

[0052] Fasudil hydrochloride API: Kunming Pharmaceutical Group Co., Ltd., batch number 201201-01.

[0053] 2. Experimental method

[0054] 1. Solution preparation

[0055] 1.1 0.1% formic acid-water solution: precisely pipette 1ml of formic acid into 1000ml of water, and mix well.

[0056] 1.2 Diluent: Measure 300ml of water and 700ml of acetonitrile, mix well.

[0057] 1.3 Reference substance stock solution (50ng / ml): Take about 10m...

Embodiment 2

[0103] Embodiment 2, adopt the inventive method to carry out quality analysis to Fasudil hydrochloride

[0104] Fasudil hydrochloride raw material comes from Kunming Pharmaceutical Group Co., Ltd., with a total of 6 batches, and the batch numbers are 201201-01, 201201-02, 201201-03, Y170508-2, Y170509-2, Y170510-2.

[0105] The preparation of need testing solution (0.5mg / ml): get fasudil hydrochloride crude drug 10mg, accurately weighed, put in 20ml measuring bottle, dissolve and dilute to scale with diluent, shake up, as need testing solution .

[0106] Get the above-mentioned need testing solution injection high-performance liquid chromatograph and use the quadrupole rod Orbitrap mass spectrometer in conjunction, record chromatogram (the collection of illustrative plates of 201201-01 batch sees Figure 4 , the collection of illustrative plates of other batches is similar to it), calculate the content of genotoxic impurity methyl 5-isoquinolinesulfonate in the test sample ac...

Embodiment 3

[0111] This embodiment is with embodiment 1, and difference is that the concentration of fasudil hydrochloride need testing solution is 0.4mg / ml, and the concentration of 5-isoquinolinesulfonate methyl ester reference substance solution is 0.1ng / ml.

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Abstract

The invention belongs to the field of medicinal chemistry analysis and particularly relates to a method for detecting methyl isoquinoline-5-sulfonate in fasudil hydrochloride. The method includes thata high-performance liquid chromatography-mass spectrum system is adopted to detect a methyl isoquinoline-5-sulfonate reference substance solution and a fasudil hydrochloride test sample solution. According to the detecting method, the high performance liquid chromatography is firstly adopted for component separation, the position of a chromatographic peak of the methyl isoquinoline-5-sulfonate inthe fasudil hydrochloride test sample solution can be determined under the chromatographic condition, the chromatographic peak of the methyl isoquinoline-5-sulfonate is effectively separated from chromatographic peak of adjacent other components, and the operation time is short; then, the mass spectrum condition is adopted to quantify a high-resolution primary mass spectrum, ppm level of methyl isoquinoline-5-sulfonate can be detected, and the limit of quantitation can reach ng / ml. Therefore, the methyl isoquinoline-5-sulfonate in fasudil hydrochloride can be effectively controlled.

Description

technical field [0001] The invention belongs to the field of pharmaceutical chemical analysis, in particular to a method for detecting methyl 5-isoquinolinesulfonate in fasudil hydrochloride. Background technique [0002] Fasudil hydrochloride is a new type of isoquinoline sulfonamide derivatives, which can dilate blood vessels by increasing the activity of myosin light chain phosphatase, reduce the tension of endothelial cells, improve the microcirculation of brain tissue, and protect ischemic brain tissue. At the same time, it can antagonize inflammatory factors, protect nerves against apoptosis, and promote nerve regeneration. Fasudil hydrochloride and its injection were launched in China in 2004, mainly for the improvement of symptoms of ischemic cerebrovascular diseases caused by cerebral vasospasm after subarachnoid hemorrhage. [0003] Impurity control is one of the important contents of drug quality control. Whether the impurities in drugs can be fully and accuratel...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/89G01N30/72G01N30/86G01N30/34G01N30/06
CPCG01N30/06G01N30/34G01N30/72G01N30/8634G01N30/89
Inventor 李宁陈云建刘世成李剑峰高宏涛
Owner KPC PHARM INC