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Method for detecting ethyl 5-isoquinoline sulfonate in fasudil hydrochloride

A technology of ethyl isoquinolinesulfonate and fasudil hydrochloride is applied in the field of detection of ethyl 5-isoquinolinesulfonate in fasudil hydrochloride, which can solve the problem of low detection limit and expensive gas chromatography mass spectrometry , easy to contaminate the chromatographic column and mass spectrometer ion source, etc., to achieve the effect of improving detection sensitivity and high ionization efficiency

Active Publication Date: 2021-04-20
HIGH & NEW TECH RES CENT OF HENAN ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the quantitative analysis method that can be used for ethyl 5-isoquinolinesulfonate is liquid chromatography mass spectrometry, and the price of this type of equipment is relatively expensive compared to gas chromatography mass spectrometry
Due to the low detection limit of this target compound, a large number of drug substance injections are required, which can easily contaminate the column and MS ion source

Method used

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  • Method for detecting ethyl 5-isoquinoline sulfonate in fasudil hydrochloride
  • Method for detecting ethyl 5-isoquinoline sulfonate in fasudil hydrochloride
  • Method for detecting ethyl 5-isoquinoline sulfonate in fasudil hydrochloride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A detection method of 5-isoquinolinesulfonic acid ethyl ester in fasudil hydrochloride, it comprises the steps:

[0039] 1) Preparation of test solution: Accurately weigh 25 mg of fasudil hydrochloride test product, place in a 20 mL headspace bottle, add 0.5 mL of internal standard solution and 0.5 mL of derivative solution, seal, shake well, and use as Test solution.

[0040] 2) Preparation of reference substance solution: with ethyl 5-isoquinolinesulfonate as reference substance and acetonitrile as solvent, a series of reference substance solutions with different concentrations containing internal standard solution and derivative solution were prepared.

[0041] The series of reference substance solutions containing different concentrations of internal standard solution and derivatizer solution, the preparation method is as follows:

[0042] Accurately weigh 10 mg of ethyl 5-isoquinolinesulfonate reference substance, place it in a 25mL volumetric flask, dissolve it w...

Embodiment 2

[0064] Example 2 Sample injection precision test

[0065] Described sampling precision is meant: get the reference substance solution that the concentration that contains internal standard solution and derivatizer solution is 0.40 μ g / mL (standard curve 100% point) continuous sample injection 5 times, record ethyl iodide and butyl iodide Quantitative ion peak area, calculate the relative standard deviation of 5-isoquinolinesulfonic acid ethyl ester by internal standard method. The results are shown in Table 3.

[0066] The peak area of ​​table 3 derivative ethyl iodide and internal standard derivative butyl iodide

[0067]

[0068] The results in Table 3 show that the RSD% of the peak area ratio of the derivative ethyl iodide and the internal standard derivative butyl iodide is 3.32%, indicating that the injection precision is good.

Embodiment 3

[0069] Embodiment 3 sensitivity test

[0070]Precisely pipette the reference substance solution whose concentration is 0.40 μg / mL (standard curve 100% point) quantitatively containing internal standard solution and derivatizer solution, dilute step by step with diluent, then measure and analyze, when the signal-to-noise of quantitative ion peak The concentration at the ratio of about S:N=10:1 and 3:1 was used as the limit of quantification and detection limit. The results are shown in Table 4 below.

[0071] Limit of quantitation & detection limit of derivatives of table 4 ethyl iodide

[0072]

[0073] The results in Table 4 show that the detection limit of the method of the present invention is 0.01 μg / mL; the quantification limit is 0.03 μg / mL. It shows that the sensitivity of the method meets the specified requirements.

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Abstract

The invention relates to a method for detecting ethyl 5-isoquinoline sulfonate in fasudil hydrochloride. The method comprises the following steps: 1) preparing a test solution; 2) preparing a reference substance solution; and 3) carrying out headspace gas chromatography-mass spectrometry determination: carrying out headspace-gas chromatography-mass spectrometry determination on a series of reference substance solutions with different concentrations, which are prepared in the step 2) and contain the internal standard solution and the derivative solution, measuring and recording the quantitative ion peak areas of iodoethane and butyl iodide, drawing a standard curve and calculating to obtain a linear equation by adopting an internal standard method and taking the ratio of the quantitative ion peak areas of iodoethane and butyl iodide as a vertical coordinate and the ratio of the concentrations of iodoethane and butyl iodide as a horizontal coordinate, carrying out headspace-gas chromatography-mass spectrometry on the test solution, recording the quantitative ion peak areas of iodoethane and butyl iodide, and substituting the quantitative ion peak areas into a linear equation to calculate the content of ethyl 5-isoquinoline sulfonate in the test solution. The method is good in stability and high in accuracy, and the detection sensitivity can reach 0.03 [mu]g / mL.

Description

technical field [0001] The invention belongs to the technical 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 antagonizes inflammatory factors, protects nerves against apoptosis, and promotes nerve regeneration. Fasudil hydrochloride and its injection were launched in China in 2004, mainly for the improvement of ischemic cerebrovascular disease caused by cerebral vasospasm after subarachnoid hemorrhage. [0003] Generally speaking, the synthesis technique of fasudil hydrochloride all takes 5-isoquinoline sulfonic acid as starting material, reacts w...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 宋寒赵振芳朱盈蕊谢亚雄李琦路任明浩朱雁
Owner HIGH & NEW TECH RES CENT OF HENAN ACAD OF SCI
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