Method for detecting 5-Isoquinolinesulfonic acid in fasudil hydrochloride

A technology of ethyl isoquinolinesulfonate and fasudil hydrochloride, which is applied in the field of detection of ethyl 5-isoquinolinesulfonate in fasudil hydrochloride, can solve the problem of 5-isoquinolinesulfonate Ethyl acetate detection method, ineffective detection, long running time and other problems, to achieve the effect of high detection sensitivity, good for safety control, and short running time

Active Publication Date: 2019-02-22
KPC PHARM INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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

Method used

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  • Method for detecting 5-Isoquinolinesulfonic acid in fasudil hydrochloride
  • Method for detecting 5-Isoquinolinesulfonic acid in fasudil hydrochloride
  • Method for detecting 5-Isoquinolinesulfonic acid in fasudil hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0041] Example 1

[0042] 1. Instruments and materials

[0043] 1. Main instruments

[0044] Mass spectrometer: AB SCIEX company, model API 4000.

[0045] Liquid chromatograph: Shimadzu company, model LC20AD.

[0046] Electronic balance: METTLER company, XP205 type.

[0047] 2. Experimental materials

[0048] Ethyl 5-isoquinolinesulfonate reference substance: Provided by Kunyao Group Co., Ltd., with a purity of 97.62%.

[0049] Fasudil Hydrochloride API: Kunyao Group Co., Ltd., batch number 201201-01.

[0050] 2. Experimental method

[0051] 1. Solution preparation

[0052] 1.1 0.1% formic acid-water solution: accurately pipette 1ml of formic acid into 1000ml of water and mix well.

[0053] 1.2 Diluent: Measure 300ml of water and 700ml of acetonitrile, and mix well.

[0054] 1.3 Reference substance stock solution (50ng / ml): Take about 2mg of 5-isoquinoline sulfonate reference substance, accurately weigh it, and place it in a 200ml measuring flask, dissolve it with diluent and dilute to the mark...

Example Embodiment

[0100] Example 2. Quality analysis of fasudil hydrochloride by the method of the present invention

[0101] The raw material of Fasudil Hydrochloride comes from Kunyao Group Co., Ltd. There are 3 batches with batch numbers 201201-01, 201201-02, 201201-03.

[0102] Preparation of test solution (0.5mg / ml): Take 10mg of fasudil hydrochloride crude drug, accurately weigh it, and place it in a 20ml measuring flask, dissolve it with diluent and dilute to the mark, shake it up, as the test solution .

[0103] Take the above-mentioned sample solution and inject it into high performance liquid chromatography with triple quadrupole mass spectrometer, and record the chromatogram (for the chart of batch 201201-01, see Figure 4 , 201201-02 batch map and Figure 4 Similar, see the map of batch 201201-03 Figure 5 ), calculate the content of genotoxic impurity 5-isoquinoline sulfonate ethyl ester in the test product according to the linear equation under item 4. The results are shown in Table 8. ...

Example Embodiment

[0107] Example 3

[0108] This embodiment is the same as Example 1, except that the concentration of the fasudil hydrochloride test solution is 0.4 mg / ml, and the concentration of the 5-isoquinoline sulfonate ethyl reference solution is 0.1 ng / ml.

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Abstract

The invention belongs to the field of medicinal chemistry analysis and particularly relates to a method for detecting 5-Isoquinolinesulfonic acid in fasudil hydrochloride. The method is that a high-performance liquid chromatography-mass spectrum system is adopted to detect a 5-Isoquinolinesulfonic acid reference substance solution and a fasudil hydrochloride test sample solution. According to thedetecting method, the high performance liquid chromatography is firstly adopted for component separation, the position of a chromatographic peak of the 5-Isoquinolinesulfonic acid in the fasudil hydrochloride test sample solution can be determined under the chromatographic condition, the chromatographic peak of the 5-Isoquinolinesulfonic acid 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 ternary quadrupole rod mass spectrum, ppm level of 5-Isoquinolinesulfonic acid canbe detected, and the limit of quantitation can reach ng/ml. Therefore, the 5-Isoquinolinesulfonic acid 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 ethyl 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 accurately...

Claims

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Application Information

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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
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